Table of Contents

Table of Contents
1.0 Purpose
1.1 Scope
1.2 Acknowledgements
2.0 Manufacture of Platinum Dioxide
2.1 Discussion
2.2 Review of alternative procedures
2.3 Equipment
2.4 Chemicals
2.5 Dissolution of Platinum in Aqua Regia
2.6 Oxidation of Ammonium Chloroplatinate to Platinum Dioxide
3.0 The Hatch-Feinstein Reduction
3.1 Discussion
3.2 Test-vessel construction
3.3 Pre-reduction of platinum dioxide
3.4 Primary reaction vessel construction
3.5 Reductive amination of P2P using Adam's catalyst
4.0 Manufacture of 1-phenyl-2-propanone
4.1 Equipment
4.2 Chemicals
4.3 Production of 1-phenyl-2-nitropropene
4.4 Reduction of 1-phenyl-2-nitropropene to 1-phenyl-2-propanone
4.4.1 Equipment construction
4.4.2 Iron Reduction of 1-phenyl-2-nitropropene to 1-phenyl-2-propanone

4.4.3 Alternative reduction procedure

5.0 Manufacture of Methylamine from Formaldehyde and Ammonium Chloride
5.1 Equipment
5.2 Chemicals
5.3 Methylamine Hydrochloride
5.4 Methylamine Solution
6.0 Manufacture of 70% Nitric Acid
6.1 Chemicals
6.2 Equipment
6.3 Discussion
7.0 Laboratory Equipment and Procedures
7.1 Fume Hood
7.2 Water Aspirator
7.3 Distillation Tips
7.4 Reference Material
8.0 Keeping Out Of Trouble
1.0

Purpose:

To describe the manufacture and application of platinum dioxide, commonly

known as Adams catalyst or platinum black, with the goal of opening
alternative synthesis procedures for the manufacture of illicit recreational
drugs. It is this writer's hope that these procedures will result in the
undermining of the Drug Inquisition, which has caused the loss of freedom for
many good people. A further goal is to demonstrate to those in law
enforcement that knowledge is, in fact, the ultimate power and that no
number of self-righteous goons with guns can defeat a resourceful and
knowledgeable mind. There is no new chemistry here; in fact, most of it is
almost 100 years old. The contribution this writer hopes he is making is in
simplifying the equipment and procedures to the point where those without
extensive chemistry backgrounds will be able to manufacture high-quality
phenethanamines in high volume to compete with the poisonous stuff one

finds on the street. The text is aimed at those who have completed a college
level organic chemistry course and have some experience and an interest in
laboratory equipment and procedures.
1.1 Scope
The following procedures will be described.
Dissolution of platinum metal in aqua regia to produce chloroplatinic acid,
then ammonium chloroplatinate.
Oxidation of ammonium chloroplatinate to platinum dioxide.
Reductive amination of P2P using platinum dioxide catalyst.
Manufacture of methylamine using formaldehyde and ammonium chloride.
Manufacture of 1-Phenyl-2-Propanone using benzaldehyde and nitroethane.
Practical manufacture of 70% nitric acid
1.2 Acknowledgements
This writer thanks Uncle Fester, whose widely read books on
methamphetamine manufacture have provided an invaluable source of
research information collected in one volume. In addition, this writer thanks
Dr. Alexander Shulgin, whose practice of the purest sort of science-that
motivated by curiosity and a deep thirst for knowledge-in the face of
government oppression has earned him my deepest admiration and respect.
This document is dedicated to Senators Orrin Hatch and Diane Feinstein,
whose tireless efforts to eliminate the vestigial remains of our civil liberties in
the cause of state expediency has pissed me off enough to take the time and
effort to produce this text. In fact, I have named the reductive amination step
the Hatch-Feinstein Reduction.
2.0 Manufacture of Platinum Dioxide

2.1 Discussion
As those familiar with clandestine drug manufacture are aware, the
traditional catalysts used in reductive amination procedures, Raney nickel
and palladium-on-carbon, are no longer available due to essential-chemical
prohibition by the anti-drug thugs. Thus the need for an alternative catalyst
which can be manufactured utilizing common materials and equipment.
Platinum dioxide has many advantages in it's application to reductive
aminations:

It can be made using common materials and easily obtainable equipment.

Reactions are performed at room temperature and at low pressure (<30 psi),
thus eliminating the requirement for simultaneous heating and agitation and
opening the door to simple high-volume manufacturing. One can easily
perform 25-30 mole reactions using a 5 gallon paint shaker for agitation.
The catalyst is reusable up to six times.
Requires a catalyst density of only 1g/mole of precursor.
Provides a product yield of approximately 1kg/g of catalyst, and a 75% moleto-mole yield from precursor-to-product (the reaction yield is 90%, the
balance being lost during processing and crystallization) when manufacturing
methamphetamine.
Is used with common ethanol solvent, eliminating odd smells and fire
hazards.
Platinum dioxide catalyst also performs well in the manufacture of
methylenedioxymethamphetamine (MDMA), but under slightly different
conditions.
2.2 Review of alternative procedures
We will focus upon the manufacture of methamphetamine due to the current
high volume requirement and the increasing attention it is drawing from the
government antidrug machine.
The best route for manufacturing methamphetamine is the direct reduction of
the hydroxyl on the L-ephedrine sulfate sidechain in glacial acetic acid using
70% perchloric acid as a promoter and 5% palladium-on-carbon as the
catalyst. Vigorous agitation, pressurization with hydrogen to 30 psi, and
heating to 90C results in an 85-90% yield of non-racemic
methamphetamine, with a 70% yield-to-product. Due to it's non-racemic
chirality, this meth is stronger than that produced by any other nonstereospecific reduction technique. Typically, this reaction is performed in a
4000ml filter flask placed into a 6 gal aluminum pot containing water. The pot
is heated on a stirring hotplate and agitation is provided by a stirring bar
magnetically coupled through the non-ferrous aluminum. A solution of 1.25
liters of glacial acetic acid, 120ml of 68-72% perchloric acid, 166g (one mole)
of L-ephedrine sulfate, and 16g of 5% palladium-on-carbon is pressurized to
20-30psi with hydrogen gas and reduced for 2-3 hours. The catalyst is filtered
out, the filtrate made basic with 50% lye solution then extracted with toluene
and stripped of solvent, the base is purified by distillation and crystallized in
acetone for the hydrochloride salt. Despite what has been written by others,
this reaction does not work with ephedrine hydrochloride because the

hydrochloride ion poisons the catalyst, whereas the sulfate ion may actually
act as a promoter (I have not tried it, but in theory sulfuric acid may be
substituted for perchloric acid as a promoter). This reaction will, however,
perform well using any ephedrine base. Due to the requirement for
simultaneous heating, stirring, and pressurization, this reaction is limited to
1-3 mole batches. In addition, the palladium-on-carbon catalyst is not
reusable without processing.
The most common current method of meth production is the direct reduction
of the ephedrine hydrochloride hydroxyl using 57% hydriodic acid and red
phosphorous in a 4-1-1 formula (4 lb ephedrine, 1 gal 57% hydriodic acid, 1 lb
red phosphorous). This is an inefficient method, yielding 55% dmethamphetamine at the very best, which has been exploited as far as it can
go due to the attention paid to the precursor and essential chemicals used in
this reaction and the increasing diversion of Chinese ephedrine supplies to
our industrious neighbors in Mexico. In it's favor, however, is the fact that one
person can manufacture 4 lb of very poisonous meth per day if they skip the
purification step. This is a perfect example of Gresham's Law at work (the
cheap bad stuff drives out the expensive good stuff).
The P2P reaction, for many years the preferred method for making
methamphetamine, requires 1-Phenyl-2-Propanone (impossible to buy, easy
to make), 40% methylamine solution (impossible to buy, easy to make), large
amounts of Raney nickel (hard to buy, difficult to make) and approximately
2000 psi of hydrogen along with simultaneous agitation and heating. There
are many limitations in this process, not least of which is equipment
construction. [This is a very limited truth, as there are many other ways of
reductively aminate P2P with methylamine which uses much more readily
available materials than Raney-Nickel/hydrogen gas /Rhodium]
The lithium-in-ammonia reduction. This is an elegant, high-yield reduction,
but it is gawdawful stinky and must be done a long way from civilization. The
volume of anhydrous ammonia required per mole of ephedrine relegates this
procedure to the low-volume category.
2.3 Equipment
The following equipment is required:
A stirring hotplate.
A 2" Teflon-coated magnetic stirring bar with a center lifting ridge. This is
simply a ridge around the center of the stirring bar that raises it above the
bottom surface, thus decreasing friction and providing for easier stirring of
thick solutions/suspensions. A 2.5-3.0" stirring bar will also be used and one
should also have a Teflon-coated stirring bar chaser which allows one to

retrieve stirring bars from solutions. This is an invaluable item for general lab
work.
1000ml and 5000ml Pyrex graduated beakers. The 1000ml beaker should be
thick-walled Pyrex as it needs to be slightly more heavy-duty. Do not use
ordinary glass or Mason jars as we will be heating it directly on the hotplate.
A jewelers oven. These ovens are available from jeweler's supply companies.
Look in the yellow pages. They typically have a meter which monitors the
temperature from 0-1200C and a rotary adjustment knob which controls the
temperature. The inside is lined with firebrick, as is the door, and there is a
small vent hole at the top. Buy one with an interior width and depth of at
least 9". They cost about $400 and can be purchased by anyone. An extra
firebrick may be required to center the oxidation vessel. Firebricks can be
found at most fireplace/woodstove stores.
One 1000ml round-bottom flask.
An 8"x8"x2" Corningware casserole dish with Pyrex top. This item is
important because it is the vessel we will use to perform the oxidation
procedure, which takes place at 520C. Ordinary glass will shatter at these
temperatures, and Pyrex does not hold up much better. Corningware will
stand up to these temperatures and heating cycles, but just barely. The Pyrex
tops that come with the casserole dish often crack or break after only one or
two reactions, so extra tops should be purchased. A ceramic or clay vessel
would be better, but are difficult to find in the correct size. The Corningware
dishes are cheap, disposable, and can be purchased anywhere.
A 4" diameter Buchner.
A 1000ml filter flask.
Whatman Qualitative 5 filter papers. Purchase the size that fits your largest
Buchner and cut to fit for the smaller Buchners. These filters will catch the
finest particles of catalyst. Equivalent filter paper is made by other
manufacturers.
A mortar-and-pestle set, medium sized. These can be found at many organic
food and food-supplement stores, as well as in children's science shops.
2.4

Chemicals

The following chemicals will be used:

Laboratory grade 37% hydrochloric acid. One can try hardware store muriatic
acid if it is 30% or better. It is unknown what the impurities in the cheap
hardware-store stuff may do to the catalyst, but many times the only

difference between laboratory grade chemicals and commercial grade stuff is

the fact that the laboratory grade chemicals have been tested to make sure
there's nothing strange in it. It may have come out of the same tanker car,
but it was tested.
One will need 200ml of 70% nitric acid in order to make aqua regia. Jewelers
can buy this in very small quantities for making aqua regia, which is required
to dissolve metals like platinum and rhodium for alloying or plating.
Otherwise, one can whip up a batch fairly easily. See Section 6.0 for
instructions.
About 3 kg of sodium or potassium nitrate. This is our oxidizer, and it is used
at a 10:1 weight ratio with ammonium chloroplatinate (which we will make). It
is also used to manufacture 70% nitric acid. Sodium nitrate is preferred, but
only because this writer has used it extensively. Use the powdered form as it
requires less grinding and seems to work better than the beaded form often
found in university labs.
About 3 kg of ammonium chloride will be used. This common salt is used for
metal preparation and making chilling solutions. It should not be difficult to
find. Try the drugstore or pharmacy.
2.5 Dissolution of Platinum in Aqua Regia
The first step is to dissolve the platinum, either in coin form or as spent
catalyst, in aqua regia to make chloroplatinic acid. This is not as easy as may
first appear. Platinum coins are especially difficult to dissolve. Left on it's own,
it could take months for the platinum to completely dissolve. Heating to just
below the boiling point of the acid will increase the activity of the acid many
times and will let the chemist dissolve his platinum coins in 3-4 days. Spent
catalyst may also be recycled, and will dissolve much more quickly than
coins. This procedure must be performed inside a properly functioning fume
cabinet or the fumes will kill you. See the appendix for construction details.
Place a 1000ml Pyrex beaker on the stirring hotplate. Place a 2" Teflon-coated
stirbar with a center ridge inside the beaker. If one is using fresh 1oz platinum
coins, gently place two of them (64g) in the beaker. There should be room for
the stirbar to turn without touching the coins. Two coins is the very most one
should attempt to dissolve in 800ml of aqua regia as additional platinum will
not dissolve and react but will remain as unreacted particles in suspension,
screwing up subsequent procedures. (If one is recycling spent platinum
dioxide catalyst, wait until after the aqua regia is made and stirring, but not
heating, is begun before adding the spent catalyst in small portions.) Add
200ml of 70% nitric acid. Add 600ml of laboratory grade 37% hydrochloric
acid. Once the platinum and aqua regia are inside the beaker, fill a 1000ml
round-bottom flask half full of cold tap water, dry the outside with a paper

towel, and carefully place it on top of the beaker. Make sure there is an airgap at the pouring lip of the beaker so no pressure builds up. This is our
makeshift condenser, designed to condense and recycle the aqua regia while
the platinum dissolves. Without the condenser, the aqua regia will quickly boil
off without dissolving much platinum. Do not fill the 1000ml flask to more
than 1/3 or full or it will become top-heavy and tip over from the vibration.
Begin heating while stirring, slowly raising the temperature over several
hours until the first signs of boiling begin. On my stirring hotplate, an 800watt
unit, the heat setting is 3.5-3.75. The solution will turn orange, and then a
very deep ruby red. Do not leave the reaction unattended for more than a
few minutes, and turn it off at night. When recycling spent catalyst, a small
amount of contaminant may appear on the surface. Let the beaker cool until
it can be handled and then filter the liquid through your 4" Buchner using
filter paper, holding the coins in place with the Teflon-coated stirbar chaser.
Do not use any metal, as it can contaminate the batch. A more porous grade
of filter paper may be used. Pour the filtrate back into the beaker with the
coins and continue the heating and stirring. It should take 3-4 days to
dissolve two coins. The variables affecting dissolution speed are surface area,
acid temperature, and stirring effectiveness.
One needs to mix up a saturated solution of ammonium chloride in distilled
water. Pour 3000ml of distilled water into a 5000ml beaker (or a 1gal pickle
jar) along with a 3" stirring bar. Place on a stirplate if available, otherwise stir
using a clean spatula from the kitchen. With stirring, slowly add ammonium
chloride to the water until it will not dissolve any more. Continue stirring
occasionally until the solution comes up to room temperature once again,
then add more ammonium chloride until no more will dissolve. Repeat one
more time. When finished, the chemist should have a room temperature
solution with a little undissolved ammonium chloride at the bottom.
Once the platinum is completely dissolved, remove the condenser flask and
allow the remaining acid to boil off until it is all gone and there remains in the
bottom of the beaker a grayish-red-black layer of ugly metallic stuff. This is
chloroplatinic acid. Be aware that the fumes created when boiling off the acid
will create large, very visible clouds of acid-laced fog if exhausted into cool,
still air. In addition, all nearby plant life will turn brown and quickly die. If
performed while a stiff breeze is blowing, this hazard is eliminated. Let the
beaker cool down, add 500ml of 37% hydrochloric acid, let it react with the
chloroplatinic acid, then boil off the acid almost to dryness. Do this three
times to remove any trace of nitric acid, boiling off the acid to dryness on the
third boil. Once cool, add small portions of ammonium chloride solution and
work it with the end of a stirbar chaser. Continue adding ammonium chloride
solution until all of the chloroplatinic acid has reacted and there are no solid
chunks left. Decant into another clean beaker or jar as the beaker fills. A

bright yellow suspension will form as the chloroplatinic acid reacts with the
ammonium ion to make ammonium chloroplatinate. Do not get in a hurry. It
can take over an hour for the chloroplatinic acid to completely react. Black
particles or other discoloration is a sign of incomplete dissolution of the
platinum. Remove the water by vacuum filtering through the 4" Buchner with
Qualitative 5 filter paper using a water aspirator or vacuum pump. This also
may take several hours. Remove the pasty ammonium chloroplatinate cake
and break it up as finely as possible using a clean razor knife in a glass bowl
or plate. It will be difficult to handle and a little sticky. At this point one must
improvise a little. I use a vacuum oven purchased at a mining equipment sale
(mines do a lot of inorganic chemistry) to gently vacuum dry the ammonium
chloroplatinate overnight at low heat. Those without vacuum ovens should
use an infrared lamp placed near the plate and be patient. Do not overheat,
as ammonium chloroplatinate will decompose. Look for any brown or black
discoloration as a sign of excess heat. Break up into smaller chunks as the
paste dries. Dried ammonium chloroplatinate is hard, granular, and dark
yellow in color.
Ammonium chloroplatinate is a convenient form in which to store catalyst, as
platinum dioxide catalyst can be extremely pyrophorric (this stuff explodes!).
Store in a cool, dry place and oxidize it as the need for fresh catalyst arises. If
one started with 64g of platinum coins (Pt, 195g/mole, 0.328mole), one
should end up with slightly less than 0.328 mole of ammonium
chloroplatinate ((NH4)2PtCl6, 443.9g/mole), or about 140g. This is enough to
make about 50g of useful catalyst, which translates to 150-300 moles worth
of reactions, or about 40-80lb of very pure methamphetamine, depending
upon how many times one is able to reuse the catalyst.
2.6 Oxidation of Ammonium Chloroplatinate to Platinum Dioxide
This is where the rubber meets the road in this procedure. We must mix our
ammonium chloroplatinate with sodium nitrate, our oxidizer, and burn it. In
the old days, when Adams invented this catalyst, they used a copper-alloy
block with a crucible and a hole drilled for the insertion of a thermometer to
measure the temperature. Our procedure isn't much better, but if Adams
could do it with crude equipment, perhaps we can optimistically expect to do
as well. At this point, your humble writer must point out that he has never
made a batch of catalyst that did not work, even though experiments were
performed over the temperature range of 480-530C. This is not due to some
extraordinary intelligence or experience. It is because this is easy to do. The
accompanying poor quality picture shows new brown catalyst on the left and
spent black catalyst on the right.
The ammonium chloroplatinate must come into "intimate contact" with the
oxidizer, according to Adams. To accomplish this, place 50g of sodium nitrate

in a layer at the bottom of your mortar-and-pestle set. Add 5g of ammonium

chloroplatinate chunks to the bed and grind until all chunks are thoroughly
blended into a homogenous yellow powder. Be thorough here, as it will pay
off in catalyst yield. Shake the mixture into the 8"x8" Corningware casserole
dish. Do this five times for a total of 25g of ammonium chloroplatinate and
250g of sodium nitrate. Do not attempt to do more than this-it makes a
terrible mess inside the oven. A safer amount is 20g, but 25g batches will
work reliably if the oven is controlled properly.
Spread the yellow powder evenly across the bottom of the casserole dish,
replace the Pyrex cover, and place the dish into the jeweler's oven. The idea
here is to place the dish so the temperature on the front meter accurately
reflects the temperature inside the vessel. If one has a large oven with the
temperature sensor in the center, adjust the position of the dish with varying
thicknesses of firebrick. If the heating element runs directly beneath the dish,
spot heating should be avoided by placing a thin firebrick across the bottom.
We are operating close to the temperature limits of the vessel material, so a
little diligence is required. The oven should be placed inside the fume cabinet
where the noxious fumes produced can be exhausted, preferably into a stiff
wind at night. Secure the latch on the oven. On my oven, the temperature
control is graduated from 1 to 10. I set the control on 3.75, having learned
the hard way that too-rapid heating will shatter the casserole dish. The
temperature will slowly climb over a period of 2.5-3.0 hours to 520C, at
which point the heating element is turned off and the chemist leaves the
oven to cool down overnight. He does not open the door of the oven, even a
crack, until the temperature is all the way down. Failure to exercise patience
will be swiftly punished with a shattered dish and a nasty mess. One should
watch the oven carefully, noting that the heating element cycles on and off
and correlating that with changes on the temperature indicator. This will
improve one's precision in controlling the oven temperature in the event one
should desire to experiment, which this writer encourages. A plume of brown
fumes should begin to rise from the exhaust hole at the top as the oxidation
begins. This usually occurs starting at 380-400C and can continue all the
way up to about 500C, but not always, and not predictably. This writer has
discovered empirically that the temperature range over which catalyst can be
successfully produced is 490-520C, with the best catalyst being made at
510C. As the meters used on these ovens are the inexpensive current-shunt
type, they are accurate to about 2%, which is about 10C either way, so
there can be as much as 20C variance in the temperature indicator from unit
to unit. In addition, the temperature sensors used have tolerances that can
stack up in the wrong direction. The point here is that your oven may read
differently than mine, so one should be observant and adjust the setting
based upon the results of the previous oxidation. If the stuff turned out burnt,
lower the temperature.

Open the door-latch of the cold oven and remove the casserole dish. Pry the
top off gently with a screwdriver, as it will be fused with white sodium nitrate
residue. Inside will be a layer of hardened sodium nitrate mixed with and
covering a layer of brown-black powder which will have spattered and coated
the inside surface. Pour some distilled water into the top and gently work it
with a plastic spoon to dissolve the sodium nitrate and free up the platinum
dioxide particles. Carefully pour the resulting liquid into the clean 5000ml
beaker. Repeat to recover the last traces of catalyst stuck to the cover. Pour
distilled water into the casserole dish until the bottom layer is covered and
break up the hard layer as gently as possible with a clean screwdriver. Work
the chunks until they are broken up into pieces small enough to handle. Using
surgical gloves, very carefully place the larger pieces into the 5000ml beaker,
rinsing one's fingers with distilled water into the beaker. Once the large
pieces have been removed, add water and work the dish until one is satisfied
as much catalyst as possible has been recovered. Add distilled water to the
large beaker until it is almost full and stir until all of the sodium nitrate has
dissolved and one is left with a dark brown suspension that gradually settles
to the bottom of the beaker. Let it settle overnight then carefully decant the
water without disturbing the catalyst layer at the bottom. Decant as much
water as possible without losing catalyst, then refill with more distilled water,
stir thoroughly for 15 minutes, then let it settle overnight once again. Do this
four times to insure all the nitrate is dissolved and removed. Successive
washings will result in the catalyst taking longer and longer to settle out,
until, on the fourth one, the catalyst may become colloidal and not settle out
completely. Using the Whatman Qualitative 5 filter paper and a clean
Buchner, filter the catalyst suspension, washing the beaker with distilled
water to catch the last grains. One should now have a layer of wet, mediumto-dark brown catalyst in the Buchner. Gently work the small cake loose onto
a small glass or porcelain plate and spread it out using a fine-tipped razorknife. Let it dry in a warm, but not hot, place. Once dry, carefully scrape the
loose powder into a clean spice bottle, which makes an ideal container. Do
not let it fall freely through the air more than a few inches as this can, and
will, result in a display of pyrotechnics as your catalyst explodes while you
watch. This is especially true when the temperature drops below freezing or
one is in a very dry area. One should now have about 11g of platinum dioxide
(PtO2, 227.09g/mole, 0.048mole) for a yield of about 85%.
Repeat the above three steps until all the ammonium chloroplatinate is used.
One should have 50-60g of catalyst in the form of a very finely divided dry
brown powder. Store in a cool, dry place and avoid static discharges. There is
some debate about whether or not this catalyst decreases in activity level
over periods of time exceeding 6-12 months. It has been this writer's
experience that the catalyst itself maintains it's activity level as long as it has
not been pre- reduced or otherwise exposed to concentrated hydrogen. There

are many other factors that can easily cause a decrease in yield or an
increase in reduction time that can be misinterpreted as a change in catalyst
activity. This catalyst is very sensitive to the level of self-oxidation or residual
acids in the P2P. In addition, slight variations in agitation effectiveness can
appear to be catalyst-related.
3.0 The Hatch-Feinstein Reduction

Application of Platinum Dioxide Catalyst to the Reductive Amination of 1phenyl-2-propanone (P2P). In this section the chemist pre-reduces the
catalyst and reductively aminates both test and production quantities of P2P.
3.1 Discussion
The prudent chemist always runs a small test batch before using fresh
chemical components, in this case either P2P, methylamine, or catalyst. In
addition, there is a requirement for a pre-reduction vessel for the catalyst.
This writer will tell you flat-out that the literature on the subject of prereduction is wrong. First of all, this catalyst must be pre-reduced in distilled
water, not ethanol. Dropping this catalyst into alcohol is an excellent way to
start a fire. Although this catalyst is gradually reduced down to platinum
during it's exposure to hydrogen, only in the very poorest of catalyst does
this occur in less than three uses. In every case, however, the catalyst
required pre-reduction. The amount of pre-reduction required varies from
batch to batch and the chemist must learn to tell from observation when the
catalyst is ready for use.
3.2 Test-vessel construction

One must construct some simple equipment in order to run test-batches and
pre-reduce catalyst in appropriate amounts.
Fortunately, the equipment can be fairly simple because we are only required
to provide agitation and low pressurization. Eliminating the requirement for
heating simplifies things immensely. As one can observe in the accompanying
picture, this writer constructed a vessel out of an old 3000ml reagent flask. It
has the advantages of being narrow, thick-walled, and having a flat top. The
bottom plate is 3/16" aluminum plate , the connecting rods are 3/16" allthread found at the auto parts store. The top plate is " aluminum plate
recovered from the scrapyard. The gauge is a -30"Hg to +30"Hg, liquid-filled,
combination vacuum/pressure unit. They cost about $30 at industrial
equipment supply stores. The pipe is common " NPT wrapped in Teflon tape.
Everything is connected together with a brass 4-way fuel block with " NPT

thread available at the auto parts store. The valves on either end are
common gas valves found at welding equipment suppliers. One can use
oxyacetylene valves as they are " NPT on one side and gas thread on the
other. This allows one to make a direct connection between the hydrogen
tank regulator and the vessel using the red hose of an oxyacetylene torch set.
The same valve on the other end is fitted with a 3/8" nipple for pulling a
vacuum. The rubber gasket used to seal the aluminum top-plate and the
bottle-top is cut from 1/8 " rubber gasket material found in the plumbing
department of the hardware store. One must adapt this design to the
equipment available. A 2000ml filter-flask can be made into an excellent
vessel by sealing off the side-nipple (hose, screw, and clamps) and using a
modified rubber stopper on the top opening.
A smaller glass vessel is also required for pre-reducing 1g batches of catalyst.
The vessel should be about 500ml or less in volume. This is necessary
because of the physical limitations of attempting to pre-reduce tiny volumes
of catalyst in a large vessel, especially considering the fact that one must
determine visually the pre- reduction state of the catalyst. The bottom plate
must be made of aluminum so a magnetic stirring bar can be used for
agitation. The unit is placed on a stir-plate, the air evacuated, then charged
with hydrogen and agitated until the catalyst is pre-reduced.
3.3 Pre-reduction of platinum dioxide
Much of the existing literature concerning Adam's catalyst describes prereducing the catalyst in ethanol and/or allowing the catalyst to pre-reduce in
situ. My experience indicates both techniques are wrong. Attempting to prereduce this catalyst in ethanol resulted in several small fires and explosions.
Attempting to pre-reduce the catalyst in situ worked on only one batch of
catalyst, which was the poorest catalyst made.
The procedure that works reliably, every time, is to pre-reduce in distilled
water. The pre-reduction process involves exposing the catalyst to hydrogen
gas under pressure, resulting in a change in both color and character of the
platinum dioxide. Carefully weigh out 1g of catalyst on a triple-beam scale.
Place the catalyst into a small (50ml) beaker and add 10ml of distilled water.
Carefully pour the resulting slurry into the small pre-reduction vessel through
a small funnel, chasing the slurry into the vessel with an additional 10ml of
distilled water. Place a small Teflon-coated stirbar into the vessel and seal by
carefully cinching down on the retaining nuts on the top plate. Make sure the
hydrogen gas valve is closed and the vacuum valve with the nipple is open.
Attach the 3/8" hose from your vacuum aspirator and pull a vacuum in the
vessel to about 25"Hg. Close the vacuum valve and watch the gauge for a
minute. If it doesn't move, your vessel is holding a vacuum. Now open the
hydrogen tank valve and increase the pressure at the second stage of the

regulator to 30psi maximum. Open the hydrogen inlet valve on the catalyst
vessel, pressurizing to 30psi. Close the vessel hydrogen valve and watch the
gauge for a drop in pressure. If there is a leak, one can find it rapidly using
dishwashing soap mixed with water in a squirt bottle. Once the vessel is
pressurized with no leaks, begin stirring as rapidly as possible. The catalyst
will be thrown against the interior wall of the vessel as it is splashed around.
Adjust the position of the vessel on the stir-plate to maximize the splash. The
catalyst will begin to turn from brown to black in color. After an additional
amount of time, small particles of catalyst will begin "sticking" to the vessel
wall, soon forming a "ring" of tiny black flakes or particles. Once most of the
catalyst is in the "flake" form and all of the catalyst has turned from brown to
black, it is pre-reduced.
Over-reduction can easily take place, and as this drastically decreases the
activity level of the catalyst and reduces it's useful life, this is to be avoided.
The catalyst will pre-reduce more quickly during warm weather, but the prereduction time varies more from batch-to-batch than with any other factor.
One should use 20ml of distilled water for every gram of catalyst. Using less
increases the chance of over-reduction while excessive water requires the
addition of more ethanol to the reaction solution to maintain homogeneity,
thus decreasing catalyst density and increasing reduction time. Typical prereduction times are 10-25 minutes.
Once the chemist is satisfied that his catalyst is pre-reduced, he makes sure
all hydrogen valves are closed and then slowly opens the vacuum valve to
release the excess hydrogen. One should keep in mind that hydrogen reacts
with oxygen to make water, with an accompanying release of energy--one
should be careful when opening hydrogen gas valves into an atmosphere
containing oxygen. Once the pressurized hydrogen has been released, it is
time to move the catalyst to the reaction vessel. The best way to do this is to
partly fill the pre-reduction vessel with 95% ethanol, then pour the slurry into
the reaction vessel using a funnel. Repeat until all the catalyst is picked up.
The chemist is now ready to make his product.
3.4 Primary reaction vessel construction

The design of one's primary reduction vessel should be tailored to the batch
sizes and the quality of agitation one desires.
This writer constructed an adequate reaction vessel using a section of 8"
stainless-steel pipe found at the scrapyard along with some stainless plate
and threaded fittings (see pix).

In addition, a rocker was constructed using common steel plate, a gearmotor,

and some pulleys purchased at the hardware store. A cyclic rate of 100 RPM
was chosen arbitrarily (I guessed) and provision made in the design to allow
one to swap pulleys and change the cyclic rate. A throw(rock) of 3" was
determined to be the most one could expect given the motor torque (32 in-lb)
and the weight of the vessel when fully charged (about 10lb). The motor used
is a gearmotor from a scrapped copier which one can readily find at
electronics surplus houses along with the required capacitor for less than
$100. A new gearmotor of the proper size will cost 4-5 times that much.
These are very useful, reliable motors that this writer uses for many
purposes. Try to find ones with a machined face so they can be quickly
mounted to brackets, etc. The resulting rocker provides a rocking rate of 110
rpm and completes a reaction in six hours.
Our stainless reaction vessel has an internal capacity of 7000ml, of which
only 3500ml is used when fully charged with a 6.5-mole batch. This batch
size was selected because of equipment and time restrictions-one can
squeeze a 3500ml reaction into a 5000ml round-bottom flask for solvent
stripping and the resulting 900g of methamphetamine base divides
conveniently into two 450g portions for crystallization, which will take about 4
hours to perform. This is a full day's work for one person, resulting in 2lb of
product.
An improved reaction vessel can be constructed using a paint shaker for
optimum surface-area creation. These units hold one-gallon paint cans,
which, when full of paint, weigh much more than our reaction solution,
eliminating concerns about exceeding any weight limitations on the machine.
One may have a reaction vessel made which will fit into the machine clamps
and have the following properties; 1) it will be constructed of thin-wall 316
stainless steel and stand up to 100psi when sealed and will not collapse when
a 29"Hg vacuum is pulled (this means a round body and thick ends), 2) it will
have a threaded opening about 1.5-2" at one end to pour stuff into, and, 3) it
will have an internal volume of at least 4000ml. The best way to do this is to
have a machine shop roll a sheet of 0.065in 316 stainless sheet into a
cylinder and then weld the seam. End pieces are cut from 0.375in 316
stainless and tig-welded to our thin-wall pipe. Prior to welding to the cylinder
body, one end-piece is drilled out and a 1.5" stainless coupling with NPT
thread is welded on. The unit is then pressure tested to 100psi and vacuum
tested to 29"Hg. The threaded coupling is fitted with a bushing that allows a
gas fitting to be attached. Use Teflon tape to seal all threads, including the
gas fittings. Leaks must be avoided. This one gallon (4liters) vessel can hold
3500ml of reactants with ease, resulting in the same product volumes as one
obtains using the rocker. The improvement comes in the vigorous agitation
provided by the paint shaker; by making sure that the hydrogen inlet hose

rises straight up from the vessel to avoid losing reactants into the hose, the
reaction will reach completion in 3 hours instead of 6 using the same catalyst
density of 1g/mole. Using very little ingenuity, one can obtain a paint shaker
that holds 5-gallon pails and construct a reaction vessel which will do 30-mole
batches in a few hours, resulting in about 10lb of finished product after
processing. The batch can be processed in 22- liter glassware by reducing the
ethanol volume slightly, but will require a high-volume vacuum source to do
the distillation. The main drawback to doing huge batches is that if one
makes a mistake, he has just blown a whole lot of very valuable precursor
material. The prudent chemist does not bite off more than he can chew up in
one day.
3.5 Reductive amination of P2P using Adam's catalyst
While the catalyst is pre-reducing, the chemist must prepare a Schiff's base
from his P2P and methylamine solution.
For a 1-mole test batch using 1g of catalyst, one pours 150ml of 37-40%
methylamine solution into a 1000ml beaker along with a stirring bar. With
stirring, 134g(1mole) of 1-phenyl-2-propanone is added. This should be done
inside the fume cabinet to avoid the strong smell of decaying fish that
accompanies methylamine solutions. Cover the beaker with a clean shop rag
while stirring continues. In a separate container, measure out 250ml of 95%
ethanol. 95% ethanol can be purchased as very strong vodka under various
brand names (Everclear?), but my favorite source of ethanol is found in
almost every supermarket and drugstore. It is called Rubbing Alcohol
Compound. This is very different from Rubbing Alcohol, which is the trade
name for isopropyl alcohol. Rubbing Alcohol Compound has replaced
isopropyl alcohol on grocery shelves because the ethanol subsidies provided
by the feds allow the use of cheap subsidized ethanol instead of the more
expensive isopropyl alcohol. Rubbing Alcohol Compound is 93% ethanol along
with 2% ethyl acetate or some other denaturant that makes you sick if you
drink it. Fortunately, the denaturants do not affect our reaction and now one
has an inexpensive source of reaction solvent upon which no liquor taxes are
paid. This writer has tried every brand available in my area and they all
worked just fine. In a serious pinch, the chemist can use methanol instead of
ethanol, although the reaction will take three times as long to complete with
a similar yield. When the catalyst is ready, slowly add, with stirring, enough
ethanol to clarify the solution. This should take about 125ml for a 1-mole
batch, leaving 125ml to use in retrieving the catalyst from the pre-reduction
vessel. Add the clarified P2P/methylamine solution to the reaction vessel and
rinse the beaker with a dash of ethanol, adding the rinse to the reaction. One
should now have a reaction vessel containing 20ml of water, 250ml of
ethanol, 150ml of methylamine solution, and 135ml of P2P for a total volume
of about 550ml. Keep this number in mind when designing a larger reaction

vessel. Seal the reaction vessel, pull a 25" vacuum using a water aspirator,
pressurize to 5psi with hydrogen, pull another 25" vacuum, and then
pressurize to 25-30psi with hydrogen. Do not pull a vacuum harder than
25"Hg or the methylamine will boil off. Check for leaks. If no leaks are found,
begin the agitation by turning up the stirring to full blast.
Agitation is important because it creates surface area. For the reaction to
take place, the catalyst, a molecule of our Schiff's base, and an atom of
hydrogen must come into contact simultaneously. Since we are dealing with
solid, liquid, and gas phase materials, this can be difficult. The splash, or
agitation, is the single most important physical variable affecting this
reaction. The more surface area one can create, the better the chances are of
our three reactants meeting and making meth.
At this point, one would like to know if the reaction is proceeding correctly
and at what rate so one knows when the reaction is done. Our
pressure/vacuum gauge along with our gas valve will provide this
information. Once the reaction vessel is pressurized to 30psi, close the
hydrogen valve and begin the agitation; the reading on the pressure gauge
should drop over a short period of time. In my test vessel, a pressure drop of
10psi occurs in 11-16 minutes, depending upon how good the agitation is.
Yours may be different. Once the pressure has dropped 10psi, open the
hydrogen valve again and re-pressurize to 30psi. By precisely recording the
amount of time it takes to cause a pressure drop of 10psi, the chemist can
tell whether the reaction is proceeding or stopped for some reason, how well
(quickly) the reaction is going, and when it is done. This can be vital
information if something is going wrong. Typically, a 1-mole reaction in this
writer's test vessel will use a 10psi gulp of hydrogen every 13 minutes for 10
gulps, and then begin to slow down as the reaction begins to have difficulty
finding unused reactants. A total of 18 10psi gulps of hydrogen are required
to complete a 1-mole batch in my test vessel. The last hydrogen gulp takes
well over an hour to finish, with a total elapsed time of about 4-6 hours to
complete the reaction. Using a known volume and pressure, one can
calculate how many pressure drops it will take to use up a mole of hydrogen.

With the reaction done, the chemist pours the reaction solution into a 1000ml
beaker and rinses the vessel out with a little ethanol, adding the rinse to the
beaker. One must now remove the catalyst before processing. This is
accomplished by using a small(2") Buchner along with Qualitative 5 filter
paper and filtering into a 1000ml filter flask. Capture the remaining particles
of catalyst in the beaker with ethanol. At this point, the chemist must be on
his toes because the catalyst in the Buchner will catch the alcohol on fire if it
is not quickly quenched. This is done by pouring a layer of distilled water over

the catalyst and allowing the vacuum suction to pull it through, taking the
alcohol with it.
One must always keep in mind that this catalyst is very pyrophoric, meaning
it will burst into flames or explode at the slightest provocation. Things one
should never do with this catalyst at any time, but especially once it has been
pre- reduced, are; 1) allow it to fall freely through the air for more than a few
inches, 2) allow it to come into intimate contact with flammable solvents such
as ethanol, methanol, etc., and, 3) expose it to open flame. We have forced
hydrogen atoms into the lattice structure of the platinum dioxide crystals,
and that hydrogen reacts with oxygen both in the air and the platinum
dioxide (reducing it over time to platinum), and this reaction creates heat
which will catch things on fire. A static charge of sufficient intensity, such as
that picked up when falling freely through dry air, will cause the catalyst to
explode, although not with an intensity that will damage anything but one's
dignity.

Now that the catalyst is removed, pour the filtrate into a 1000ml roundbottom (RB) flask and distill the ethanol and methylamine off until the
temperature reaches 90-92C. Turn off the heat, attach an empty receiving
vessel, then slowly apply a vacuum by gradually closing the bleeder valve on
the water-aspirator system. When the temperature has dropped and the
vacuum is down to 28-29"Hg, turn on the heat again and vacuum distill off
the residual water until the condenser is clear, which will occur between 5060C. Remove the heat and allow the remaining meth base to cool a little.
With fresh boiling stones and a clean receiver that has been weighed, reapply
the vacuum and distill the meth base over a 10C range. Adjust the vacuum
using the bleeder valve so that the meth base distills over at 95-105C. Meth
base is a clear, colorless liquid. If it is anything but clear and colorless, it
contains contaminants. The accompanying picture shows the result of a 6.5
mole batch, which produces about 900g of meth base.
A one-mole batch of P2P with 100% conversion would result in 149g (one
mole) of methamphetamine base, but the typical yield is 90-93%, resulting in
134-140g of base. Meth base will quickly react with carbon dioxide in the air
to form the carbonate, so it is advisable to crystallize the base as soon as
possible. Crystallization is performed by adding 450g(3 moles) of meth base
to a 1000ml Pyrex beaker and placing the beaker on a stirring hotplate.
Carefully drop in a Teflon- coated stirring bar and begin stirring. One now
adds 37% hydrochloric acid in 15ml portions. A graduated 15ml test-tube
makes an ideal dispenser. A great deal of heat is generated as the acid reacts
with the meth base and will result in boiling if added too quickly. Add 15ml of
acid at intervals of 1 minute until 19 portions (285ml) have been added, then

add acid in smaller portions and watch the color carefully. If the meth base
was clean to begin with, it will turn light pink when the pH reaches 3-4. Test
with pH strips(Colorphast 0-14 strips) or a meter. Stop adding acid when the
pH reaches 3.

Now we must boil off the water contained in the acid, as water solvates meth
very efficiently. Turn the heat on the hotplate to 4.5 while stirring continues
and place a thermometer that reaches 150C into the beaker on the bottom.
Over the next 1.5 hours, the temperature will climb to 110C where boiling
begins, then gradually rise as the water is boiled off. When the temperature
reaches 130C, turn off the heat and remove the thermometer. Using a
dishtowel, grip the beaker with both hands and quickly pour it into a 5000ml
plastic bucket containing 4.5 liters of acetone which has been frozen for 2
weeks. Retrieve the stir-bar with a chaser, replace the lid and return to the
deep freeze for 1 week to allow complete crystallization. Clean, freshly
distilled acetone will retain about lb of product the first time it is used,
which is why one should recycle one's acetone. Alternatively, one can pour
the hot methamphetamine hydrochloride into a 5-gal plastic bucket
containing 4.5-gal of acetone that has been frozen for about a month (it takes
a long time to pull the heat out of a large mass). The meth will crystallize the
instant it hits the frozen acetone, although about 25% will remain in the
acetone and must be frozen to crystallize.

Paradoxically, dirty meth crystallizes better than pure meth because the
crystals quickly grow around a particle of impurity, forming nice large, hard
crystals. The meth crystals are filtered out using a large Buchner, two 4000ml
filter flasks, and a high-volume vacuum aspirator. An 18cm porcelain Buchner
will hold a little over 1 lb of filtered product. Do not use Qualitative 5 filter
paper for this filtration. This writer has found that the filters used in milk
processing equipment are ideal for meth harvesting. A lot of money has been
spent by the dairy industry over the years figuring out how to quickly filter
solids out of mixed-phase solutions. These filters will allow liquids, both water
and oils, to pass freely while trapping the finest solids, making them ideal for
rapid filtering. The problem with the fine paper filters is that oil-water
mixtures plug them up very quickly. Milk filters do not have this problem and
they are easy to find, cheap, and suspicionless. One will need to cut-to-fit, but
this is a small inconvenience. A suitable high-volume filtering setup can be
easily made using 5 and 20-liter buckets, a round plastic plate, and some
glue. This writer was fortunate enough to discover a large Buchner being
used as a planter by a nice lady in my neighborhood. Happily paying the lady
for a replacement, the retrieved treasure holds over 2lb of product and makes

the chemist's life much easier. The point is that one can find useful
equipment almost anywhere. Pure meth is more difficult to crystallize, and
results in a light, flaky white product with a mild scent of marzipan (actually
benzaldehyde). Empty the product into a large cake tray and let the acetone
evaporate in the fume cabinet for a day or two, separating it as it dries.
This product may be cut with powdered niacinamide (vitamin B3) at a 4:1
ratio (20% cut) to make a product that burns clean and is water-soluble. Do
not use vitamin B-3 tablets which contain insoluble buffers that burn dirty.
4.0

Manufacture of 1-phenyl-2-propanone

The manufacture of P2P utilizing benzaldehyde and nitroethane is described.

We will be using a two-stage procedure involving the Cope modification of the
Knoevengel reaction and an iron-acid reduction procedure. The chemistry of
this procedure has been described by Uncle Fester in his Secrets of
Methamphetamine Manufacture, 3rd ed., thus we will concentrate on scaling
up the reaction to the point where it can be used for very high-volume
manufacture.
4.1 Equipment
The following equipment will be required.
A rigid-base heating mantle with dual-element controls that holds a 22-liter
round-bottom triple-neck.
A 22-liter, 3-neck, round-bottom reaction flask
A 45/50 to 24/40 glass fitting adapter
A Dean-Stark trap
Two 30cm West condensers
Several 5-liter and 20-liter plastic buckets
Fabricated equipment described below
4.2 Chemicals
Benzaldehyde
This is our basic starting material. One mole of benzaldehyde weighs close to
100g and has a density close to 1g/ml. Since we will be performing 25-mole
reactions, we will use 2500ml of benzaldehyde per reaction. All other reactant
quantities are derived from this figure. Purchase the chlorine-free type if

available, but the standard product works fine. Store in a cool, dark place.
Benzaldehyde will auto-oxidize somewhat over time, but is nothing to get
excited about-this stuff will keep. The oxidation product is benzoic acid, which
takes the form of well-defined white crystals at the bottom of the container.
Try not to get any of the crystals into the reaction. They won't kill it, but will
reduce the yield. Benzaldehyde has a strong odor of marzipan. It can be
vacuum-distilled in order to clean it up, but has a tendency to bump
vigorously at vacuum levels that are high. Benzaldehyde has been relatively
easy to obtain until recently.
Nitroethane (EtNO2)
This is the material we will react with the benzaldehyde molecule in order to
produce 1-phenyl-2-nitropropene. It supplies the carbon sidechain and nitro
group that are required to produce the nitrostyrene. EtNO2 is a clear,
pleasant- smelling liquid which boils at 114-115C, has a molecular weight of
75.07g/mol, and a relative density of 1.05. It distills nicely without vacuum.
Since we will be providing a 5% excess of nitroethane in order to ensure there
are enough molecules available to combine with the benzaldehyde, we will
require 26.25 moles of nitroethane((26.25mol x 75.07g/mol)/1.05), or
1,875ml for each batch. One can use the industrial grade nitroethane, but it
must be washed and distilled before using. To clean it up, pour about 3000ml
of nitroethane into a 4000ml separatory funnel, add 500ml of distilled water,
shake thoroughly, allow the water to separate to the top over a 24-hour
period, then drain the nitroethane and distill it, discarding anything that
comes over below 110C. It is important that the nitroethane be clean. One
should be aware that nitroethane has become a high-suspicion product
because it sounds much like nitromethane, which is the booster that was
added to the Oklahoma City bomb. Do not confuse the two.
n-butylamine (n-BuNH2)
This is our catalyst. Do not use "sec-" or "tert-" butylamine, as they will not
work(the "n-" means "straight- chain"). In addition, because n-butylamine is a
very strong base which reacts with carbon-dioxide in the air and almost
anything else it contacts, one must insure that the catalyst is clean. The best
way to do this is to distill it. Do this inside a fume cabinet as this stuff is very
ugly. Don't breathe it and don't touch it. One must wrap the stopper or cork
on the distillation rig in Teflon tape to prevent it from being eaten. The
amount of catalyst used in our 25-mole reaction is nominally 20ml/mole, but
experience has shown that the actual amount is closer to 23ml/mole, so one
should purchase an amount that will provide a volume of 25ml/mole of
benzaldehyde. The actual amount must be determined by observation and
adjusted accordingly. The use of catalyst that is not pure will result in a
drastic reduction in yield.

Ferric Chloride (FeCl3)

This innocuous chemical is used in our reduction reaction in small quantities
as a "steerer", which modifies the reaction equilibrium in the direction we
desire. A few kilos of this can do a lot of reactions.
Catalytic Iron Powder (Fe)
Used in the reduction procedure, the iron reacts with hydrochloric acid to
produce hydrogen gas. Due to the requirement for good dispersion during the
reduction, the use of a fine mesh powder is necessary, either 80 or 100 mesh.
A coarser 60 mesh powder can be used, but may result in some problems if
the stirring system is inadequate. The reaction requires 200g of iron powder
for every mole of 1-phenyl-2-nitropropene that is reduced. Since we will be
performing 20- mole reductions, each reduction will require 4000g of iron.
Muriatic acid (HCl)
This is simply dilute hydrochloric acid, usually about 28-32% as compared
with 37% HCl. It works just fine, however, and has the advantage of being
available at almost any hardware store. A volume of 750ml of 37% HCl is
required for every mole of 1-phenyl-2-nitropropene that is reduced, resulting
in 15 liters of acid required for every 20-mole reduction. It has been this
writer's experience that the more dilute muriatic acid performs just as well as
the stronger stuff in the same volume.
Methanol (MeOH)
This is used as a solvent when processing the yellow nitropropene crystals.
Purchase methanol which has not been diluted with water-some of it is only
60% methanol. Keep it in the deep freeze.
Toluene
This is our solvent for the Knoevengel reaction. It is available in every paint
store, although many companies are relabeling their solvents with house
names so the narcs don't hassle them. Use the "UN" number, which must be
on every container, to identify the product. Or just ask. Most paint store
employees don't know the difference between toluene and neoprene and will
happily tell you anything you want. Our Knoevengel reaction requires 200ml
of toluene for every mole of benzaldehyde, or 5000ml for every reaction.
4.3

Production of 1-phenyl-2-nitropropene

Set up the 22-liter RB in the heating mantle. Add 10-20 PTFE(Teflon) boiling
stones to the vessel. Through the wide center neck, add 5000ml of toluene,
2500ml of benzaldehyde, and 1875ml of nitroethane, in that order, with

stirring. Have the fitting reducer, Dean-Stark trap, and a West condenser
greased up and assembled nearby. We will need to assemble the pieces
quickly once the n-butylamine is added. Using a wooden dowling rod as a
stirrer, quickly add 550ml of n-butylamine with stirring. The reaction mixture
will turn from clear to a milky consistency as a Schiff's base and a molecule of
water are formed(the water turns the solution milky). Assemble the fitting
reducer, the Dean-Stark trap, and the West condenser on top of each other
and plug the two side necks. Attach a fitting to the top of the condenser and
run an exhaust line into your fume cabinet. Start the water running through
the condenser. Wrap some aluminum foil around the top half of the reaction
vessel and the Dean-Stark trap to avoid excessive cooling.
Turn on both heating elements and set the temperature controls at 20%. At
this setting it will take a long time to heat up the solution. After one has some
experience with this reaction, one can start out with the heating mantle at a
higher setting(70% for 20min on my rig). One must be aware that we are
using only a small West condenser for cooling and that it takes very little
extra heat to blow material out the top. On my equipment, the proper setting
is 18%--20% is too hot. Be very careful with the heat. The idea here is to boil
the solution just hard enough to reach the bottom of the condenser where the
water-toluene azeotrope can condense out into the Dean-Stark trap and be
removed from the reaction solution. This occurs at 85C.
Once the reaction reaches the condenser, the water will begin to accumulate
rapidly. For a 25 mole reaction, 25 moles of water will be created and must be
removed for the reaction to reach completion. This writer's Dean-Stark trap
holds 25ml of water, resulting in a total of 18 full water-traps to complete a
25-mole reaction. Use a piece of paper and make a mark every time the trap
is emptied. The water will come over rapidly at first, taking only a few
minutes to fill the trap, and then slows down as water molecules get harder
to find. The reaction should take about five hours to complete, but one should
not use time as a definitive indicator. One will do much better at judging the
quality and state of one's reaction by observing the color of the reaction
mixture. As the water is removed, the solution will begin to turn a light
orange color and deepen as the reaction nears completion. The use of too
much catalyst, n-butylamine, will cause the reaction to polymerize to some
degree, resulting in a dark brown solution color, poor quality nitropropene
crystals, and a greatly reduced yield. Unfortunately, this reaction is very
sensitive to the quantity and quality of the catalyst. Too little catalyst will
reduce the yield significantly and too much will burn(polymerize) it. This
writer advises that one do test batches of 1 and 5 moles in order to home in
on the exact amount of n-butylamine required. If the reaction is allowed to
continue once all the water is removed, it will begin to polymerize, so one
should carefully watch the color of the reaction solution and keep careful

track of the amount of water removed. Even if all of the theoretical amount of
water has not been removed, if the solution color starts turning dark, pull it.
Turn off the heat, allow the boiling to subside into the vessel, remove the
condenser and Dean-Stark trap, then carefully lift the vessel out of the
heating mantle and place it on a plastic bucket inside the fume cabinet.
Leave it to cool down to room temperature overnight.
We will now strip the toluene solvent from the solution by performing a
vacuum distillation. One needs a high-volume adjustable vacuum source in
order to perform this distillation. Do not use a vacuum pump to strip solventsit's hard on the pump and poses a high fire hazard. Always use an aspirator
when vacuum-distilling solvents. Your typical university aspirator that runs off
40psi of water pressure is not adequate to pull a decent vacuum in a large
volume, let alone an adjustable vacuum. We will be working with a system
volume of about 27 liters. Attach two West condensers in series and support
them carefully with tri-grips or wooden blocks with grooves cut into the tops.
Attach a 5000ml round-bottom flask that has been marked at the 5000ml
level. We will use this mark to determine when we have finished. Once
completely assembled, turn on the heating mantle and set the controls at
30%. Once again, the reader's system/equipment will be slightly different
from mine and he must make some minor adjustments. The idea here is to
distill off the toluene at a temperature high enough to allow the condenser to
liquefy the toluene so it doesn't get sucked into the vacuum system where it
can cause damage. About 26-27"Hg or thereabouts will produce a distillation
temperature range of about 40-60C, which is hot enough to be condensed
out by water at 10C. One should not attempt to distill off the toluene at a
normal atmosphere because the added heat quickly polymerizes the product
as the toluene is removed. One must also make sure one has removed ALL of
the toluene; even a small amount will prevent the crystals from forming or
will produce poor quality crystals that polymerize rapidly in the open air.
Since we started with 5000ml of toluene, we need to strip off at least that
much. Use a mark on the receiver.
Once the toluene has been stripped off, turn off the heat, disassemble the
equipment, and then pour the hot, orange liquid remaining in the vessel into
two 5-liter plastic buckets, filling each of them to about 1/3 full and then
covering. Quickly rinse and wash the big reaction vessel with methanol
before the residue adheres to the walls. Let the liquid nitropropene cool for a
few hours, then cover and place at the bottom of the freezer overnight. In the
morning, the crystals will be formed and we must remove any unreacted
material and contaminants. To accomplish this, pour about one liter of
methanol which has been frozen for a week or two into one of the buckets
holding the solid mass of crystal and break up the mass with a big
screwdriver. The yellow nitropropene crystals are only slightly soluble in cold

methanol, but the undesireable reaction remnants are very soluble, so we will
dissolve the gunk while leaving the crystals intact. Once converted into a
slurry, filter through a Buchner. Do the same to the other bucket. Empty the
bright yellow crystals into a large cake tray and let them dry. Once dry, place
into a 5gal bucket, cover, and place in the deep freeze. Left in the open air,
the nitropropene crystals will polymerize in about one month. Stored in the
freezer, these crystals will keep nicely for at least two years.
The yield on this reaction is not 100%, as stated in other literature. The
theoretical yield is 79%, but the best this writer has achieved is 74%, with
70% being the average. Since one mole of 1-phenyl-2-nitropropene weighs
168g, one should end up with 25 moles x .7, or 17.5 moles of nitropropene
crystals which weigh about 2940g. This writer advises that the chemist make
and store all of his yellow nitropropene crystals before proceeding to the next
step.
The chemist may wish to experiment with other strong bases in order to find
an alternative to n-butylamine, which is rare enough to be a choke point.
4.4

Reduction of 1-phenyl-2-nitropropene to 1-phenyl-2-propanone

4.4.1 Equipment construction

This procedure is the most difficult described. Not because the reaction is
difficult to perform, but because of the equipment one must build in order to
make it workable. The problem is one of scale; A two-mole reduction can be
performed in 5000ml glassware using a heating mantle and standard stirring
equipment. To reduce a 20-mole batch requires ten times the volume, 50
liters, a controllable heat source, and scaled-up stirring equipment.
Additionally, we will perform a steam-distillation in order to extract and purify
the final product, which will require a large condenser. We will want this
condenser to also operate in the reflux mode during the reaction in order to
keep the acid from boiling off and killing everything. To make matters worse,
we will be working with 15 liters of muriatic acid, which means everything
must be made of stainless-steel. Fortunately, this equipment is neither
difficult nor expensive to construct. One needs to either own and be proficient
with a TIG welder or find a shop that can do the work. If one must use shops,
spread the work around. They will all ask what it's for-simply tell them that
you have a non-disclosure agreement and would lose your job or contract if
you told them. Or make up your own story.

Our reaction vessel will be a 50-liter stainless stock-pot found at the

kitchen/restaurant supply. It must be stainless, and not aluminum. Highquality stainless pots have aluminum-clad bottoms for better heat transfer-

this is good. They will all be fabricated of thin-wall stainless, but look for the
most heavy-duty pot you can find. This pot is the weak point in our
equipment because the boiling hydrochloric acid will eat through the wall of
the pot in 5-7 reactions, after which a new pot must be purchased.
In order to seal the pot, a flange must be welded onto the pot rim and
provision made for attaching and sealing a top. This is done by carefully
measuring the diameter of the pot rim and fabricating a flange to fit. We will
be using a 3/16" polypropylene "O" ring for a seal and a series of bolts on the
outside to accomplish the sealing and attaching. The ring should be about 2"
wide, with the bolts(3/8" stainless hardware) on the outside and a 1/16" x
3/16" groove machined into the flange face about " from the inside rim.
Polypropylene O-ring material can be found at most good hydraulics shops
and machine shops. We will be using 1/8" diameter or 3/16" diameter O-ring
material, whichever is available. Buy enough for several rings, as they wear
out. Our flange must also be flat to within 1/16" so the top isn't warped. Do
not weld the flange to the pot until the top-plate has been fabricated.
We also have a requirement for knowing the temperature of the reaction at
all times. In order to do this, one must either weld a stainless bushing into the
side of the pot that fits an industrial thermometer or create a fitting in the top
through which one can insert a thermometer long enough to reach the
reaction solution. Good luck finding a thermometer that long. This writer
chose the bushing-in-the-side method with mixed results-the temperature
indication worked great but the boiling acid eats the thermometers and the
bushing weld creates a weak point which the acid attacks and eats through
after only three reactions. Covering the weld completely with fast-drying J-B
Weld after each use doubled the lifespan of the pot to six reactions. I'm sure
someone out there can think of something better. A Teflon- coated pot would
be nice.
Now that we have the beginnings of a reaction vessel, we will need a heat
source. Fortunately, one can find propane- powered barbeques almost
anywhere, including the heavy-duty one pictured, which is more than
adequate. A 30lb propane tank is good for about three reactions.

Now we must design our top-plate, which is fairly complex. The first step is to
have a matching circle of 3/16" thick stainless-steel cut and drilled to fit the
flange so they can be bolted together. Next, we must provide for a Teflon
bearing in the middle. This writer designed a bearing machined from 3" Teflon
round stock. Since the gearmotor used to turn the stirrer has a " driveshaft,
the bearing consisted of a " hole in the middle and a " wide outside
shoulder machined down to " depth. This results in a " thick bushing wall,

which has held up without problem. Using these dimensions, a center-hole of

1.5" diameter and four 10-32 threaded holes on the outside rim are required.
It is advisable to have the Teflon bushing machined first and then fitted to the
top. A shaft clearance of 0.003-5 works well. Unfortunately, one must know
the diameter of the motor driveshaft in order to design the bearing. Many
motors have 5/8" driveshafts which will operate perfectly with the above
bushing design by simply enlarging the center hole, leaving a 3/8" bushing
wall. The stirring shaft should be standard 316 stainless round stock with a
flat machined at one end to make attaching the vanes easy.
The importance of vigorous stirring cannot be overemphasized. If too much
iron remains on the bottom, it can cause a runaway reaction, which you will
regret. To avoid this, keep the iron in suspension and the reactants moving.
This writer has determined experimentally that about 150 rpm is a good
speed for stirring, but this can vary depending upon the effectiveness of the
stirring vanes. The vanes on the reaction vessel shown were a simple plate
welded onto the bottom of the shaft, insuring that it did not contact the
thermometer shaft inserted through the pot wall.
Now that we have a bearing and driveshaft, we must design a bracket that
will hold our gearmotor firmly in line with the bearing and driveshaft. The
picture above shows the gearmotor without the bracket, as the unit has been
disassembled for storage. The reader will be left to his own devices in this
bracket design since there is little chance that your gearmotor will be exactly
like mine. Since there are two more attachments which must be placed on
the top cover, one should locate an adequate gearmotor early on in the
design and then wait until the end to fit the motor and bracket. The motor
should have a shaft speed of about 150 rpm and a torque of 32 inch-pounds
or better, keeping in mind that the more reaction mixture being turned, the
more torque is required.
A 2" stainless nipple must be welded to the top plate to accommodate the
condenser and it's fittings. In addition, a threaded " hole must be placed in
a location near the outside of the top plate. A " NPT stainless nipple screws
in here and is attached to 5/16 Tygon tubing leading to the acid reservoir. This
is where the acid enters the reaction vessel.

The condenser and its fittings are fairly straightforward. Four 5' sections of "
thinwall stainless tubing are grouped within a 2" diameter circle and welded
into a flat flange with outside boltholes. Use " bolts for strength and a thick
rubber gasket. The outside waterjacket is 4" thinwall truck exhaust tubing
which is light and cheap. It is fitted with " NPT bushings at each end for
water circulation. It is sealed at the end with another flange, leaving 6-9" of

tubing sticking out the end. The waterjacket should be 4' long. Use
dishwasher hoses found at the hardware store that have " NPT thread on
one end and hose thread on the other for circulating water through the
system. The condenser will need to be supported with chains due to it's
weight when full of water. In order to use the condenser in both distillation
and reflux modes, another flange must be fabricated which can be moved
around in combination with standard pipe fittings. A combination of 2"
stainless "T" , a 2" plug, and a 6" long nipple with an angled flange of about
20C on the end worked well for this writer. The adapter flange must mate
well with the condenser flange to avoid leaks.

The following diagrams show how the condenser is configured for both
distillation and reflux modes:
A container to hold and dispense the muriatic acid is required. This writer
uses a small(5gal) plastic garbage can with a Tygon tubing siphon hole drilled
just above the acid line. A 1/8" stainless-steel flow valve is required to control
the flow of acid into the reaction. These valves may be found at industrial
supply houses like W.W. Grainger, etc. One should use only Tygon tubing as
most other types will soon harden and crack.
4.4.2 Iron Reduction of 1-phenyl-2-nitropropene to 1-phenyl-2-propanone
Pour 15 liters of clean tap water into the vessel. Follow this with 4000g of
catalytic iron, 3400g (20mol) of 1-phenyl- 2-nitropropene and 40-50g of ferric
chloride. Assemble the top with the condenser in the reflux mode, start the
water running through the condenser, begin stirring, and fire up the propane
burner. Watch the thermometer and turn off the heat when the temperature
reaches 90C. Slowly add muriatic acid in small doses over a 2-hour period.
Watch the top of the condenser for signs things are getting out of hand. This
reaction needs to be performed in a small shed or other outbuilding with
good ventilation. Install a heavy-duty (500+cfm) exhaust fan in the shed. The
reason for this is that the fumes from this reaction are very corrosive and if
the reaction goes into runaway, one will want to abandon the shed for awhile
as the fumes clear out. A total of 15 liters of muriatic acid is added. Once all
of the acid has been added, allow the stirring to continue for another 2 hours
before going on to the next step.
We now must extract our P2P from the nasty black mess inside the reaction
vessel. We will do this through steam distillation. Disconnect the condenser,
flange, and "Tee", leaving the 2" nipple open. The stirrer should remain
turning. Next, quickly pour in about 4 liters of saturated lye solution that has
cooled off overnight. Some heat and steam will be generated as the lye
neutralizes the muriatic acid. Assemble the Tee, flange, and condenser in the

distillation mode and start the water flowing through the condenser. Place a
20 liter bucket under the end and fire up the propane burner to high.
Discontinue stirring. Distill over the water and P2P until the bucket is full,
then turn off the heat.
The yield for this reduction is 75% no matter how badly one thinks he has
blown it, so we should expect to obtain 15 moles, or a little over 2000g of
P2P. Since P2P has a density close to that of water, this works out to about 2
liters of product.
We must now extract the P2P from the water, purify it, and store it for later
use. This is accomplished by pouring 3000ml of water/P2P into each of two
4000ml separatory funnel. One then adds about 300ml of saturated lye
solution to each and shakes vigorously for 3-5 minutes. This is done to insure
there is no residual acid which can, and will, poison the catalyst when used.
After a thorough shaking, 400ml of methylene chloride is added to each
separatory funnel and shaken vigorously for 2-3 minutes. Methylene chloride
is an easily obtainable solvent for most plastics. Check the plastics supply
shops that sell buckets, sheet plastic, etc. Since methylene chloride is heavier
than water, it will pick up the P2P and carry it to the bottom of the sep funnel.
This takes some time, however, so one must not get in a hurry. This writer
allows the separation to sit for 6 hours before draining the bottom layer into a
one-gallon wine bottle, or even better, an amber glass bottle. Cut a square
out of a plastic baggie and use it for a seal between the bottle-top and the
cap. Add another 400ml of methylene chloride, shake vigorously, and let it
settle out again for 6 hours before draining. This is good enough, go on to the
next batch. When finished, one should have 3-4 gallons of methylene
chloride/P2P solution.

We will now recover our methylene chloride solvent for reuse and distill the
P2P. Use a 5000ml round-bottom vessel and distill over the methylene
chloride from 39 to 60C. Return the solvent to it's container and continue
until there is only about 2000ml of P2P left in the vessel. Add boiling stones
and vacuum distill over the remnants of the methylene chloride and water
until it is clear that only P2P is left. Using a clean receiver and fresh boiling
stones, distill over the P2P at 105-115C. Do not distill at a temperature lower
than 105C or the P2P will carry contaminants over with it, the contaminants
being darker colored. P2P is a clear, pale-yellow liquid that smells like cat
piss. P2P will auto- oxidize over a period of weeks if left at room temperature,
so put it in the freezer until ready for use.
One can use toluene to extract the P2P from the water, but it must be
vacuum-distilled and the separation will be to the top instead of the bottom

like methylene chloride. It takes about the same amount of time to separate
as when using methylene chloride.
4.4.3 Alternative reduction procedure
For those unable or unwilling to construct the admittedly large number of
mechanical items described above, there is an alternative reduction
procedure that the reader may or may not find more convenient. This
reduction, gleaned from Dr. Alexander Shulgin's wonderful book PIKHAL, uses
glacial acetic acid instead of muriatic acid to create hydrogen by reacting
with catalytic iron. It also cleans up with water and eliminates the steam
distillation step used above. The downside is that, as described, it takes a
much larger volume of acid to reduce an equivalent amount of nitropropene.
It may be possible to reduce the amount of acid required, and I leave it those
interested to develop it further.
Place a 1000ml Pyrex beaker into a pan of water and rest this on a hotplate.
Add 140ml of glacial acetic acid and 32g of 80-100 mesh catalytic iron. Heat
to about 85C, just below the point where white salts begin to appear, then
add 10-15g of 1-phenyl-2-nitropropene crystals dissolved in 75ml of glacial
acetic acid. Add slowly, allowing a vigorous reaction free from excessive
frothing. Continue heating for 1.5 hours after the addition. The surface will
crust up, turn whitish, and climb the walls of the beaker. Remove from heat,
mix into 2000ml of clean water. Add enough concentrated lye solution to
neutralize the acid, then extract with methylene chloride and distill exactly as
above. One can scale this up by using a bucket made from polypropylene (try
Chevron Delo 400 oil buckets). These tough buckets will stand up to 100C
temperatures without deforming. Or one can use a stainless pot either plain
or Teflon coated. Glacial acetic acid has a strong vinegar smell which
disperses rapidly when heated, making for an odor problem hard to disguise.
But since there is no power required, one can do this in the woods
somewhere. This procedure was designed by Dr. Shulgin to reduce the
nitrostyrene associated with MDMA, so it can be used for both Meth and
Ecstasy if one can find a supply of piperonal. The reader will find that most of
the procedures described herein apply to the manufacture of both products.
This writer has tried this procedure with excellent results, obtaining a 75%
yield of a very pure and colorless P2P.
5.0
Manufacture of Methylamine from Formaldehyde and Ammonium
Chloride

The use of phenylacetones as precursors to Meth and Ecstasy require

methylamine to complete the reaction. Fortunately, it is fairly easy, if time
consuming, to manufacture. Both formaldehyde and ammonium chloride are

easily obtainable chemicals used extensively in industry. One can divert

formaldehyde from taxidermists and ammonium chloride from many plating
shops and even the drugstore. Once again, we have a two-step procedure;
the first making methylamine hydrochloride crystals which are stored in the
freezer until used, and a purification step where the methylamine is collected
and diluted.
5.1 Equipment
To perform this procedure we will need the following equipment.
A rigid-base 10-liter heating mantle with dual controls.
Two 10-liter round-bottom 3-neck flask
Three 2000ml RB flasks.
A 30cm West condenser.
A 500ml dropping funnel.
A 75cm dual-surface reflux condenser with 24/40 joints(bottom male, top
female)
Several clean 5-liter and 5-gal buckets with tops.
A fabricated condenser capable of condensing ammonia (bp -33C). This
condenser is fabricated using a 1 gallon paint can and a section of " brake
line found at the auto parts store. About 24" of brake line is carefully coiled
into a spiral that fits inside the paint can. An exit tube about 2" long and an
entrance are brazed to the can. There must be no leaks at the bottom. Also,
the coiled brake line must not have any section that is crimped or runs
"uphill" - this can cause a serious backpressure problem. When filled about
1/3 with methanol or ethanol and chilled with dry ice, this condenser will be
at -75C, which is cold enough to condense ammonia. Wrap the paint can
with pipe insulation and duct tape. Without the insulation, the dry ice must be
replenished at intervals short enough to be distracting. This writer attached a
mounting handle but later discovered that it is much easier to simply set it on
a table or bench of the proper height. Do a test run with alcohol and dry ice
to see if any leaks appear when the brazing is rapidly chilled. Check to see
that water runs smoothly through the condenser without any backpressure.
This is not a piece of equipment one wants to test as it is used.

In addition to the dry ice condenser, we will need to circulate ice water

through a reflux condenser in order to condense out any water vapor that
may accompany the methylamine gas. This writer purchased a perfectly good
circulating chiller at a mining equipment sale that pumps -20C antifreeze
solution. Otherwise, one can make a perfectly acceptable chiller out of
aquarium pumps and a 10-gallon Coleman ice chest. Connect two aquarium
pumps together in parallel so if one pump fails in the middle of the reaction
the other can continue on until the procedure is finished. Drill holes in the top
of the cooler for the pump cord and circulating lines. Add a layer of water on
the bottom and drop in several bags of ice. As the ice melts, add more. This
will give us about a 1C circulating solution. If a colder solution is desired, one
simply uses cheap plumbing antifreeze that won't freeze at -30C and chills it
with dry ice instead of water ice. The pumps may become unreliable at the
reduced temperature.
5.2

Chemicals

To make a useful amount of methylamine, the following is required.

10-20 gallons of 35-40% Formaldehyde
10kg Sodium hydroxide (lye)
Distilled water
A 40lb block of dry ice, wrapped in newspaper and stored in a good ice chest.
About 40lb of ice cubes or block ice from the supermarket
40-50kg of ammonium chloride. Industrial grade ammonium chloride is
normally mixed with a little calcium chloride to keep it from clumping up and
hardening and is called "treated" ammonium chloride. The calcium chloride
does not affect the reaction, so one can use the cheap industrial 50lb bags.
5.3

Methylamine Hydrochloride

Set up the 10-liter rigid base heating mantle inside the fume cabinet. We will
be generating some formaldehyde gas which one does not want to breathe.
Charge the reaction vessel with 3kg of ammonium chloride and 6 liters of 3540% formaldehyde. The ammonium chloride will not dissolve, so stir it with a
section of wooden dowling. Attach a 30cm West condenser, a vacuum takeoff,
and a 2000ml receiver RB flask. Lead a short section of plastic tubing from
the vacuum takeoff to a small pail of water. Use a clamp to place the end of
the tube just under the surface of the water. Some of the gas generated will
be absorbed by the water; the rest will go out the vent. Place a one-hole
rubber stopper with a thermometer in one of the side holes on the triple-neck
so the solution temperature can be easily read. The chemist then turns on the

heat, setting the controls on 70% full-scale for a short time. When the
solution temperature reaches 60C, reduce the heat controls to about 25%
and slowly bring the temperature up to 100C. The ammonium chloride will
now start to dissolve, and can be aided with some quick stirring with a
dowling rod. As the solution reaches 70C, a little gas will begin bubbling in
the water pail. As the temperature climbs towards 100C, a lot of gas will be
generated, causing pressure inside the vessel. The pressure builds up
because of the back pressure created by the West condenser, which is too
small. In fact, the condenser is the limiting factor in this reaction, otherwise
one would use a 22-liter setup and double the volume. This writer has
performed this reaction in a 22-liter rig and does not recommend it. Those
familiar with methylamine manufacture will be wondering why a pot of oil
warmed to the correct temperature is not used; the answer is that this writer
discovered that the solution temperature can be held at 104-106C using a
carefully controlled heating mantle. One will need to play with the control
adjustments a little, but it is not difficult. If the chemist experiences
difficulties holding a stable temperature, simply go back to the oil pot
method. Reduce the heat to about 15% when the solution temperature
reaches 100C. Once the solution stabilizes at 105C and the gas no longer
bubbles in the water pail, the chemist can apply an aspirator vacuum at 1530 minute intervals over the next 5 hours. At the end of 5 hours, turn off the
heat, remove the triple-neck from the heating mantle, and let it cool down
overnight to room temperature. The cooling causes a lot of ammonium
chloride crystals to precipitate out of solution. Filter out the crystals, saving
them in a separate bucket for later reuse, and save the light yellow filtrate in
another bucket. Repeat this procedure several more times until a 20-24 liter
bucket is full of liquid.
Next, set up the 10 liter triple-neck in the same manner as before and add
about 7 liters of the accumulated intermediate-stage liquid. Set the heating
mantle to about 30% and apply an aspirator vacuum of -28"Hg using a
bleeder on the vacuum system. One should be careful to thoroughly grease
all fittings with Dow-Corning High Vacuum Grease or it's equivalent to prevent
glassware freeze-ups. The chemist now patiently distils water and acid out of
the mixture until solids begin to come out of solution and strong "bumping"
begins to occur inside the reaction vessel. This can take 5-6 hours or longer.
At this point, turn off the heat, disassemble the rig, and pour the contents of
the reaction vessel into a bucket inside the fume cabinet. Leave overnight to
cool down to room temperature, at which point there will be another large
slug of ammonium chloride crystals to filter out. This time, however, a little
methylamine hydrochloride will be mixed in with the ammonium chloride.
Because methylamine hydrochloride is very hygroscopic, the salts may be
gooey. Filter through a Buchner, keeping the recovered salts in one bucket
and the yellowish liquid in another. Repeat until there is enough liquid in the

second-stage bucket to proceed to the third stage. One should be getting the
idea now that one can increase the throughput in the system by simply
setting up another 10-liter rig and processing in parallel. By organizing the
separate stages properly, one person can produce about 80 liters of 40%
methylamine in 9 weeks if one is dedicated. This is enough methylamine to
make 175lb of pure methamphetamine.
In the third step, we use the second-stage liquid we have collected and pull
more water and acid out of the solution using a vacuum of 26-27"Hg, which is
slightly lower than the vacuum used during the second stage. The vacuum
setting is important because if the vacuum is too strong it will induce
"bumping" inside the reaction vessel and if it is too weak, not enough water
will be pulled out to give us good quality crystals that do not melt the instant
they contact moist air. Pull as much water as possible out of the solution
before the methylamine hydrochloride crystals precipitate out of solution and
strong "bumping" begins, then pull the reaction and let the hot mixture cool
overnight. Using a clean Buchner, filter out the methylamine hydrochloride
crystals thoroughly, then dump them into a 5 gallon bucket that has been
resting in the freezer for a few days. Methylamine hydrochloride crystals are
whitish platelet-type crystals. Keeping the crystals in the freezer where it is
too cold for water to remain in the air prevents the crystals from picking up
water from the air and melting. Throw out the residual thick golden liquid.
Repeat the procedure until one has accumulated a full 5-gal bucket of frozen
crystals, which is the amount that one can turn into methylamine solution in
one day.
5.4

Methylamine Solution

In this step we will mix methylamine hydrochloride and sodium hydroxide to

release methylamine gas, which is then condensed with dry ice-/alcohol,
allowing us to collect pure methylamine liquid and store it in a water solution.
Before one can proceed, one must do some preparatory work to make things
go smoothly. About 8 liters of 50% sodium hydroxide solution must be
prepared the night before. In addition, a one gallon bottle (used wine jugs)
containing 2 kg of crushed ice should be placed in the bottom of the freezer
several days ahead of time. We will need to dilute the liquid methylamine
with distilled water unless one intends to manufacture Ecstasy, in which case
one will want to mix the pure methylamine with ethanol that has been frozen
for a week or so and store it in the deep freeze. Methylamine/ethanol will not
keep long as the methylamine will eventually boil away even in the freezer,
but it is much safer than storing pure methylamine by itself. The
methylamine/alcohol solution should be used within a week.
Methylamine/water will keep well for years if kept cold.

One should be aware that this step can be very dangerous to life and liberty.
Done improperly, this procedure can, and will, result in extremely stinky and
poisonous methylamine gas filling the structure and pouring out into the
street where everyone within a mile will smell it. The building will stink until it
is torn down and the unlucky chemist who experiences this will also stink of it
for a long time. One must be sober and paying close attention while
performing this procedure.
To set up the equipment, one places a 10-liter heating mantle on the floor
near the fume cabinet so any loose fumes will get sucked out. Place a clean
triple-neck into the mantle. Mount a 75cm dual-surface reflux condenser in a
tri- grip attached to a 36" lab stand. Attach the chiller lines with the input at
the bottom and the output at the top and start up the chiller pump. The top
of the reflux condenser should be within inches of a table or benchtop. Place
the methylamine condenser on the bench and connect it to the condenser
using a section of Tygon tubing and a pigtail that fits a 24/40 glass joint. Do
not use rigid connections between the different mechanical assemblies. A
pigtail can be made from a section of glass tubing and a 24/40 plug for those
with some experience with glass. The exit end of our paint-can condenser is
connected with Tygon tubing to a two-hole rubber stopper that fits snugly into
a 24/40 glass joint. Inserted into the stopper are a 4" section of glass tubing
and a 3" section. Attach the Tygon to the longer section. Cut a section of
plastic tubing that leads from the short stopper tube to the inside of the fume
cabinet. This is our vent. Next, carefully weigh three 2000ml RB flasks and
write it down somewhere, identifying each flask with a piece of duct tape
around the neck. It is important to be able to determine exactly how much
methylamine one has made when it comes time to dilute it with water. Do not
use markers on the flasks as they will disappear with alcohol-use duct tape on
the neck. Next, place a 36" lab stand and ring (about 6-8") near the bench
and our methylamine condenser. Use a 5-liter plastic bucket wrapped in
insulation on the sides and place it at a height where the 2000ml receiver
flask will sit in it nicely without requiring a long section of tubing between the
condenser and the receiver. Hook the bucket handle over the top of the lab
stand for safety, then attach a tri-grip around the neck of the 2000ml
receiver. The receiver must be held rigidly in place or it will float and bob
around in the bucket when we add alcohol and dry ice. The receiver must be
kept at -75C or the methylamine will boil away on us. Methylamine has a
boiling point of -6C, so this stuff will boil away even when it's kept in the
deep freeze. We must also insure that our stopper will not pop out of the
receiving flask by accident so one buys some Velcro strips at the variety
store, slides a narrow strip between the glass tubes on the top surface of the
stopper and uses another strip wrapped around the receiver neck, once the
stopper is in place, to trap the ends and tie the entire works together. Tapes
and other chemical-based bonding materials become fragile at -70C. Lastly,

charge both the paint can and bucket with methanol and slowly chill them
down by adding chunks of dry ice, one at a time, until they no longer quickly
boil away but remain solid at the bottom. The paint can should be about 75%
full and the bucket filled to a point at least halfway up the receiving flask. We
are now ready to rock and roll.
Using a wide-mouth funnel and a piece of wooden dowling, shove
methylamine hydrochloride crystals from the freezer into the triple-neck until
it is no more than 1/3 full. Attach the reflux condenser to the triple-neck and
place the 500ml dropping funnel into one side neck. With the stopcock
closed, charge it with 50% lye solution. Using a funnel quickly add 400g of
dry sodium hydroxide to the main reaction vessel. Quickly plug the neck with
a glass plug. As soon as the lye contacts the methylamine crystals it
produces methylamine gas and sodium chloride(salt). After an initial burst,
which one can watch run into the receiving vessel, the reaction will subside.
Now is a good time to check and insure that all fittings are tight and there is
no blockage in the condenser, which can be disastrous. Next, open the
stopcock and allow the lye solution to stream in. It can be difficult to know
when too much lye has been added because there is a delay before the
reaction reaches a peak, so it is recommended that one proceed slowly,
carefully watching the receiving flask for signs of too much liquid coming
through. Methylamine is a clear liquid with a density of about 0.7. Keep the
paint can and receiver bucket charged with dry ice and the chiller with water
ice while lye solution is added at intervals. After an addition, wait until the
condensation subsides before adding more lye. Eventually, adding more lye
solution will not produce any more liquid methylamine and we must boil the
remaining methylamine out of the solution of water, salt, methylamine, and
dimethylamine. The remaining methylamine is now in a water solution, which
we would prefer not to happen, but there must also be enough water to
dissolve the salt and hold the dimethylamine in solution, so do not cut back
on the water used in the lye solution. Turn the heating mantle to 50% and
wait, keeping things cold as you do. Over the next two hours the remaining
60-70% of the methylamine will boil up through the reflux condenser, where
the water and dimethylamines are condensed out, and then through the paint
can and into the receiver. Watch the reflux condenser for signs of salt
accumulating on the glass. This is an indication that there is not enough
water in the solution, so let the boiling subside and quickly add a liter or so of
distilled water before continuing the distillation. When no more methylamine
comes over, or it is reduced to just a drop every several seconds, the batch is
done. Turn off the heat and let things cool off for about 20 minutes until the
boiling has totally subsided. During this period, detach the 2000ml receiving
vessel and very, very carefully take it to the fume cabinet to be weighed.
Keep in mind that if one should drop and spill the liquid methylamine, it will
immediately boil into a gas, will probably kill the clumsy chemist, and will

definitely make one's lab the center of attention for weeks to come. Don't
drop it! Carry it in a frozen bucket(not a warm one). Once the methylamine
has been weighed inside the fume cabinet, lower a clean thermometer into
the liquid and leave it for several minutes until the temperature comes up to
-30C. This will let any liquid ammonia, which we do not want, boil away
leaving only pure methylamine. Weigh it, subtract the weight of the flask, and
divide the weight in grams by 0.7 to determine the volume. 1000g of
methylamine will occupy about 1400ml. Very slowly and carefully add this
first batch of methylamine to the 1-gal wine jug containing 2kg of crushed
ice. There may be considerable fuming, in which case one should stop, stuff a
rubber stopper(do not use glass) into the methylamine receiver and place the
whole works into the freezer for a while.
Fortunately, one only has to perform this ugly chore once. Once we have a
quantity of methylamine solution we know is 40%, one can simply add
enough distilled water to accommodate the next batch and throw it into the
deep freeze. The diluted methylamine solution will not freeze, thus allowing
one to simply add methylamine liquid to the solution to bring it up to the
required concentration. The formula is simple: equal volumes of distilled
water and pure methylamine liquid will result in 40% methylamine solution.
Depending upon the exact amount of crystals in the triple-neck, one should
have between 900g and 1200g of pure methylamine liquid. For those
manufacturing MDMA, add 100ml of pure methylamine to 250ml of ethanol
that has been in the freezer for a week or so. This reduces the water content
of the MDMA reductive amination, improving the yield.
Now that the first batch is complete, the chemist quickly sets up the other
triple-neck and repeats the procedure. Once the chemist has some
experience, he can do four batches in a single day if he starts early.
6.0

Manufacture of 70% Nitric Acid

Nitric acid is an essential chemical required for making aqua regia. It is also
an essential ingredient in the manufacture of nitric ester explosives, which
makes it a closely watched chemical. Jewelers are able to purchase very
small amounts (50ml) to make aqua regia for dissolving gold, platinum, and
rhodium. Some plating operations use nitric acid. Fortunately, 70% nitric acid
is easy to make.
6.1

Chemicals

One will need to acquire the following chemicals.

Concentrated (98%) sulfuric acid H2SO4. This acid is used extensively in

industry, the most visible use being as battery acid when diluted.
Sodium Nitrate. This is also a fairly closely watched chemical due to it's
application in explosives, but is so widely used in industry that it is fairly easy
to obtain. One can also use potassium nitrate in equivalent molar quantities.
Look in the drugstore.
Dry ice. A 20lb block will do nicely; chip into small flakes when used.
A bag of rock salt and several bags of crushed ice.
6.2 Equipment
A 2000ml RB flask
A 1000ml RB flask
A 30cm West condenser
A single-element 1000W electric hotplate from the hardware store.
A medium-sized kitchen pot. The 2000ml RB flask must fit into the pot.
A lab jack for raising and lowering the hotplate and kitchen pot. A suitable lab
jack may be constructed from a scissors-type car jack that has been
modified. A 10"x10" flat top is welded on the top, a circular steel plate is
welded on for height adjustment, and a nut is welded onto the back bottom
surface that will accept a standard lab stand shaft. This is necessary to
suspend the 2000ml flask containing our reactants.
A 3-4" diameter tube about 30cm long (cut to fit). This tube will be fitted
around the West condenser, plugged at the lower end, and filled with dry ice.
It can be either plastic or cardboard (mailing tubes). Make sure the condenser
will fit inside the tube.
A 2-liter plastic bucket or other container in which the 1000ml RB flask will fit
comfortably.
A controllable vacuum source.
6.3

Discussion

This is an easy procedure to perform, allowing one to make 400ml of 70%

nitric acid in one day. The basic idea is to vacuum distill over the nitric oxide
created by the reaction of sulfuric acid with sodium nitrate, condense it into a
liquid with dry ice, and then drop it into distilled water to capture and dilute
the resulting acid. The final step is to boil off the excess water, leaving about
200ml of very clean acid from each batch. The tricks to making this reaction
work are a controllable vacuum source and precision control of the heat

source.
Set up the lab jack with the hotplate and pot resting on the top surface.
Suspend the empty 2000ml RB flask above the pot with a tri-grip. Position it
so the bottom of the flask is clear of the pot. Also make sure that the pot can
be raised to a point where the flask will touch the bottom of the pot.
While the flask is bottomed out in the pot, add enough vegetable oil (Wesson
Oil works) to reach about 1" from the top rim of the pot. Lower the lab jack,
hotplate, and pot. Wipe the 2000ml flask clean with a paper towel and
remove. Turn on the hotplate to a medium setting. We wish to heat the oil to
90-100C and no hotter, so measure it with a candy thermometer and adjust
the hotplate setting accordingly. We now have a precision heat source that
can be applied and removed very rapidly by raising or lowering the lab jack.
We must now prepare our condenser. Seal off one nipple of the condenser
with a short piece of plastic tubing that has been sealed on one end by
melting the plastic together. Fill the condenser wall with isopropyl alcohol.
Seal off the remaining nipple with another section of plastic tubing. Attach
the vacuum takeoff and insert into the tubing. The top end should be
positioned so the 24/40 joint is even with the top of the plastic tube. When
positioned correctly, stuff a little pink insulation into the bottom opening and
seal the bottom end of the tube with duct tape. The vacuum takeoff should
be the only thing protruding. Attach the stillhead. Fill the tube with chips of
dry ice and seal with a little pink insulation material. One will need to
construct some custom supports for the tube-a couple of pieces of wood with
"V"s cut into them works nicely, especially if mounted to a bottom plate for
rigidity.
Next, pour 300ml of distilled water into the receiver flask and position it with
a tri-grip and stand so it rests inside our small plastic bucket when attached
to the vacuum takeoff. Add cold water to the bucket, then add crushed ice to
keep the solution cool-much heat will be generated as the nitric oxide drips
into the distilled water. Add a layer of rock salt on top of the ice to further
reduce the temperature.
Add 365ml (685g) of sulfuric acid to the 2000ml RB flask. Then 600g of
sodium nitrate is added in small portions while swirling the acid. Do this
inside a fume cabinet. There will be no visible reaction. Mount well above the
heat source. Assemble all of the glassware and attach the vacuum hose with
the bleeder valve open so there is no vacuum. Slowly close the bleeder valve
and bring the vacuum down to 25-26"Hg on the vacuum gauge.
One must be aware that excessive heat will cause foaming and the nitric
oxide to come over too fast to condense. One should slowly raise the oil pot
until it barely contacts the reaction vessel. Be prepared to quickly lower the

pot if excessive boiling occurs. Watch the drip-tip of the vacuum takeoff;
liquid nitric oxide should drip into the distilled water at a rate of 1 drop per
second, maximum. Any faster than this will result in overheating the dilute
acid and suck much nitric oxide into the vacuum system. It will take 2-3 hours
to complete the reaction. During this time, one must replenish the dry ice
supply in the tube. Use a flour scoop to carefully add to the tube. There
should be 500-600ml of liquid in the receiver when done.
The next step is to remove the excess water from the acid solution in the
receiver. This is done by simply boiling the liquid in a normal distillation
setup. Distill over water until the temperature climbs to 118-120C. What is
left in the vessel is very pure, clear 70% nitric acid. Store in a cool dry place
that is dark. It will keep for several years.
If one's nitric acid becomes discolored, simply distill it.
7.0

Laboratory Equipment and Procedures

Unless one has spent many hours doing organic syntheses, there are many
lab techniques and procedures that that will be unknown. This section
attempts to cover some of the basics applicable to clandestine labs.
7.1

Fume Hood

One must have a fume cabinet, period. Fortunately, they are easy to build.
This writer constructed an integrated fume cabinet/lab that fits on a single
sheet of plywood. Note the plastic sheeting used to seal the enclosure when
noxious fumes are present. Not shown is the exhaust fan that runs
continuously. Use a fan that moves at least 250 cfm of air.
7.2

Water Aspirator

A high volume aspirator is required for many of the procedures described in

this document. Although industrial strength aspirators can be purchased,
they can also be constructed from common pipe fittings found at the
hardware store. Shown in the accompanying photograph is this writer's
aspirator. There is a lot of cut-and-try involved in building a homebrew
aspirator, so purchase one if possible. Also required to complete an aspirator
system are a pump supplying 50-70 psi of water pressure and a reservoir of
cold water. The pump can be a common 1/3 HP jet pump wired to a switch in
the lab. These pumps are inexpensive, but are only good for about 200 hours
of hard use, so keep a spare handy. The water reservoir must hold sufficient
volume to prevent rapid heating of the water and be able to absorb solvents

and fumes. A good reservoir size is about 100 gallons or two fifty-gallon
drums connected together at the bottom and filled to 2/3. Water temperature
is very important. The colder, the better. In sub-freezing temperatures, just
add some plumbing antifreeze and one's aspirator will pull a mighty vacuum.
Unfortunately, as the water temperature rises, so does it's vapor pressure,
and this imposes a limit on the vacuum one can pull. To reduce the vapor
pressure of the water, lower the temperature with a block of ice from the
freezer.
Another essential component of the system is the vacuum trap. The trap
keeps one's mistakes during distillation from ruining the rest of the
equipment. Placed between the aspirator and the vacuum hose, it collects
any liquids not condensed into the receiver. One can be made using a 1-qt.
Mason jar. Using a drill press, carefully drill two holes in the top that are just
big enough to accept the base of a 3/8" brass nipple. Braze the nipples to the
top. Using a gasket, seat the top on the jar. Screw the top down firmly and
attach the vacuum lines (Use 3/8" reinforced hydraulic hose, as this size fits
the nipples on vacuum-takeoff glassware and doesn't collapse under a good
vacuum). Place the vacuum trap somewhere it won't get bumped; this writer
built a 3-sided wood box lined with insulation. This is because the Mason jar
will easily implode under a good vacuum. Check for leaks and use some
pliable external house caulking to fix it. It is a good idea to change the water
in the aspirator system daily, as solvents will attack the plastic pump
impellors.
The next requirement is for a vacuum distribution system. The accompanying
picture shows the vacuum input from the right, a distribution hose on top that
attaches to glassware at the other end, a 0-29" Hg vacuum gauge, and an
industrial strength 1/8" bleeder valve. A more suitable bleeder valve is a
needle valve with a 0.050 aperture. The entire assembly is located inside the
fume cabinet. The vacuum inlet at the right comes from the vacuum trap and
may be replaced as required with a vacuum pump hose.
7.3

Distillation Tips

Below are some tips that will make vacuum distillations go smoothly.
Always use Dow-Corning High Vacuum Grease or it's equivalent on glass
joints. Use sparingly and keep glass joints clean.
Use Teflon (PTFE) boiling chips. They typically come in 1 lb. Cans. Use
liberally, add fresh boiling stones each time the vacuum is broken or the
liquid cools down.
Wait until the vacuum is stabilized before applying heat, then use the
minimum heat required.

Maintain a 30C temperature differential between the water flowing through

the condenser and the condensate. The condensation line in the condenser
should be between and 2/3 the way down the condenser.
Don't fill the distillation vessel more than halfway full. You can cheat a little
bit on this one. Another don't is "bumping"; this is easily recognizable and if it
starts, stop the distillation immediately. Some heavier compounds like P2P
and benzaldehyde are naturally "bumpy", so one has to exercise some
judgement.
Don't get in hurry when doing large volume distillations; the condenser
throughput rate is fixed and adding more heat won't speed things up but will
send some of one's distillate into the vacuum system.
7.4

Reference Material

The following books are essential to any clandestine lab.

Merck Index
This handy volume provides one with all the essential data on most
compounds, including molecular weight, density, boiling and freezing points,
common usages, and references pointing to manufacturing techniques.
Uncle Fester's Secrets of Methamphetamine Manufacture, 3rd and 4th ed.,
Loompanics.
These comprehensive books provide the references and good pointers for
those reading between the lines. In reading these books, one should bear in
mind that if one is a little too accurate in his technical descriptions, one could
find one's ass in a prison sling. Hooray for Cypherpunks!
A Chemical Technicians Reference Handbook.
This is a valuable reference for solvent characteristics and lab procedures.
A college level Organic Chemistry textbook for a reference to common
reaction mechanisms.
8.0

Keeping Out Of Trouble

If one can observe all of the following tips, one might be able to retire to a
legal occupation with a good head start.
Work alone and keep your mouth shut. This is the most important advice this
writer can pass on, and the most difficult to follow. It is tempting to share
one's secret success with one's closest friend, perhaps even inviting him to

help. Unfortunately, he feels compelled to tell his wife, who is secretly

planning to leave him for a stockbroker and wants some leverage to facilitate
her stripping your friend of all his assets. Well, you get the picture. One can
crow all one wants, as I am in this document, once one has disposed of both
product and equipment.
Do not talk business on the phone. Do not even call to make an appointment
to talk. Every phone call, even local calls, are logged. Each log contains the
originating phone number, the destination phone number, the time the call
was originated, and the completion time. From this seemingly innocuous
record, Inquisition Agents can weave a pattern of times, places, and
connections that will look bad in court, even if fictitious. One can establish
secure communications using PGP encryption software and anonymous
remailers.
Never, ever, ever try to sell product while a lab is operating. This is like
juggling rattlesnakes - it's easy to get bit.
Don't make this a career. All of the career dope cookers are in prison. Decide
ahead of time how much dope you want to make, plan it carefully, do it, and
then retire. Think of it as a temporary thing one is doing to get a leg up in life.
Keep in mind that your first mistake will also be your last. There is no glory in
becoming a headline, only grief.
Acquire and store all of your essential chemicals, supplies, and equipment
before trying anything. This is the most dangerous activity, legally speaking,
one will perform. If one attracts some heat, one can wait it out without having
an operating lab to conceal. Keep in mind that the drug inquisitors do not
have the time to hang around where there are no labs to busts or assets to
seize. After a few months they will go away.
Use intermediaries to acquire chemicals, telling them you are just an
intermediary also. Never tell anyone what you are doing.
Never front product. Once one fronts product, one is assuming all of one's
customer's risks. One is better off flushing product down the drain. At least it
can't come back to bite. Do not trade for stolen property or phony money.
Don't listen to your non-chemist customers on quality issues, no matter how
emphatic or convincing they are. Users quickly build a tolerance for the
product and feel the product is no longer full strength. In addition, many
users grow to enjoy the jolt received from impurities present in much of the
present street product. This jolt is not present in pure meth.
Always act like an ignorant, low-paid middleman who has to pass messages
on to his superiors. This allows one to feign ignorance on all quality issues or

money disputes and agree with one's customer. It also provides one with
bargaining leverage, allowing one to claim that one's puny cut will be gone if
the price goes lower.
Never flash cash or start buying expensive items not in fitting with one's
usual lifestyle. If one is renting, rent a nicer place or buy a modest house. Buy
used cars and repair them to perfection instead of new, flashy cars. Invest
the profits in stocks, T-bills, and other liquid assets. Go into a legal business
and live happily ever after, knowing that one has successfully defied the
Inquisition and struck a blow for individual freedom.