Experiment 1

PREPARATION OF SODIUM CHLORIDE FOR

MEDICINAL PURPOSES

Objectives:
- Preparation of sodium chloride medicinal use from ordinary salts
- Understanding the mean of refine to remove impurities from medicinal raw materials
1. Formula and applications
- IUPAC Name: Sodium chloride
- Molecular formula: NaCl
- Molecular weight: 58.44 g/mol
*Application: Sodium chloride pharmaceutical used in pharmaceutical products such as eye
drops, infusion drugs...
* Finished product standards:
- NaCl used to make physiological saline: Content 99,0% to 100,5%
- Water used to mix: Distilled water...
- Product: Physiological saline 0.9% NaCl
2. Theoretical basis
- Step 1: Give out of insoluble impurities
- Step 2: Give out of heavy metal ions
- Step 3: Neutralize filter to pH= 4-4.5
- Step 4: Concentrate and crystallize
- Step 5: Filter the crystal
- Step 6: Dry to collect the product.
- Step 7: Make NaCl 0.9% solution.
- Step 8: Evaluate the results.
3. Materials and tools
a. Materials
Material Origin Quantity of substances
Coarse salt Vietnam 50g
Na2CO3 20% China Just
HCl 20% China Just
b. Tools

Tool Size Amount

Beaker 500 ml 2
Electric stove - 1
Buchner funnel - 1
Glass hopper - 1
Glass chopsticks - 1
Glass discs - 1

4. Experimental
- Dissolve 50g of coarse salt into 150ml of water, preliminary filter with cotton.
- The solution in the above is heated for 5 minutes.
- Use 20% Na2CO3 solution to bring to pH= 10-11, to cool, filter out the marrow, obtained
solution.
- Neutralize Na2CO3 excess with HCl solution 20% to pH = 4 - 4.5.
- Reduce the water, let it cool, and then cool it to create crystals.
- Filter the crystals on the Buchner funnel, wash once with cold distilled water.
- The resulting product is dried at 50-60C to a constant weight.
- Evaluate the results.
*Note
- Concentrated HCl is volatile, causing eye stinginess, so when mixed in the fume
hood

====================
Experiment 2
RUTIN EXTRACT FROM
STYPHNOLOBIUM JAPONICUM L.
Objectives:
- Refine rutin extracted from Styphnolobium japonicum L.
- Understand the meaning of the steps taken and the purification to remove impurities from
the ingredients for medicine.
1. Formula and applications
- IUPAC Name: 2-(3,4-dihydroxyphenyl)-5,7-dihydroxy-3-[(2S,3R,4S,5S,6R)-3,4,5-
trihydroxy-6-[[(2R,3R,4R,5R,6S)-3,4,5-trihydroxy-6-methyloxan-2-yl]oxymethyl]oxan-2-
yl]oxychromen-4-one
- Molecular formula: C27H30O16
- Molecular weight: 610.521 g/mol
*Application: Make pharmaceutical chemical materials in many products to control blood
sugar levels, protect the stomach, protect the liver, improve blood vessel function...
*Finished product standard:
- Needle-shaped crystals, pale yellow, so that the light turns dark yellow.
- 1g rutin dissolved in 8000ml water at room temperature, 200ml boiling water, 7ml boiling
ethanol, 650ml cold alcohol and 60ml hot water.
2. Theoretical basis
- Step 1: Extract rutin from Styphnolobium japonicum L.
- Step 2: Crystallization of rutin crystals
- Step 3: Wash the raw crystal
- Step 4: Refine the crystal collection of rutin crystals
3. Materials and tools
a. Materials used

Material Origin Quantity

Styphnolobium japonicum L.
Vietnam 20g
(buds and flowers)
Ethanol Vietnam 30ml
n-butanol China -
Acetic acid China -
NaOH 20% China -
 FeCl3 5% China -
Activated carbon China -

b. Tools
Tool Size Amount Tool Amount
Beaker 500ml 1 Glass rod 1
Beaker 250ml 1 UV Lamp 1
Beaker 100ml 1 Buchner funnel 1
Test tube 10ml 3 Electric stove 1

4. Experimental
a. Extract rutin from buds & flowers
- Boil 20g of Styphnolobium japonicum L. (buds and flowers) in 300ml of water for
30 minutes, filter hot quickly with cotton.
- Add 200ml of water into the residue, boil for 30 minutes, filter the heat as quickly as
above.
- Concentrate the filtered fluid until 1/2 of the original volume remains.
- The solution after concentrated to cool and scratch for crystallization.
- The mixture contains crystals that are left to cool overnight.
- Filter on the Buchner funnel to collect raw rutin crystals.
- Wash the crystals with cold distilled water 3 times, each time 10ml.
- Dry the product at a temperature of 50-60C to a constant weight.
- Evaluate the results.
*Note
- Organic solvents are volatile, so when mixing must be done in the fume hood
- When heating with alcohol must be boiled insulation

====================
Experiment 3
ANALYSIS OF RUTIN USING THIN LAYER
CHROMATOGRAPHY
1. Note
Organic solvents are volatile so when brewed must be done in the fume hood.
2. Reaction principles
a. Salt-forming reaction with NaOH

NaOH + Rutin → Na[Ru] + H2O

Na[Ru] + 2NaOH → Na3[Ru] + 2H2O
b. Complex creation reaction with FeCl3

FeCl3 + Rutin → [Fe(Ru)3/2]3+.3Cl-

3. Raw materials
Material Origin Quantity

Rutin Vietnam 10mg

Ethanol Vietnam 15ml

Distilled water Vietnam 5ml

n-butanol China 6ml
Acetic acid China 2ml
NaOH 20% China 20ml
FeCl3 5% China -
Thin layer chromatography Merk 1
Capila Tube Vietnam 1

4. Tools
Tool Size Amount
Beaker 100ml 3
Measuring cylinder 10ml 3
Chromatography column - 1
Glass rod - 1
 UV Lamp - 1
Petry discs - 1

5. Experimental
Weigh 10mg of Rutin and dissolve it into a beaker containing 15ml of Etanol. Boil
until dissolved, let it cool and divide it evenly into 3 test tubes.
• Tube 1: Add 2 drops of NaOH 20% see the appearance of orange-gold
precipitate. Continue to add reagents and find the precipitate dissolved.
• Tube 2: Add 2 drops FeCl3 5% see the solution turn blue-black.
• Tube 3: Conduct thin layer chromatography with deployment system n-butanol:
acetic acid: H2O = 3: 1: 2.5. Observe the TLC version under the UV lamp,
identify Rf = 0.3 - 0.8.
====================
Experiment 4

SYNTHESIS OF METHYL SALICYLATE

Objectives:
- Synthesis of methyl salicylate from salicylic acid, methanol, and sulfuric acid
1. Formula and applications
- IUPAC Name: Methyl 2-hydroxybenzoate
- Molecular formula: C8H8O3
- Molecular weight: 152.1494 g/mol
- Structure:

*Application: Methyl salicylate has an analgesic, anti-inflammatory effect, often used in

pain relief patches, pain relief gels...
* Product standards:
- Odorless or yellowish liquid, long-lost black aroma, almost insoluble in water, dissolved in
alcohol, ether. For the purple color with reagents FeCl3
- Density 1,178 - 1,186. Boiling point 219-224C, the refractive index at 20C: 1.535 – 1.530
2. Theoretical basis
- Esterification reaction
3. Materials and tools
a. Materials used

Material Origin Quantity

Anhydrous salicylic acid China 28g
Methanol China 80ml
Solid sulphuric acid China 8ml
b. Tools
Tool Size Amount Tool Amount
NS29 flask 250ml 1 Magnetic stirrer 1
Separating funnel 250ml 1 Electric stove 1
Condenser NS29 1 Small beaker 1

4. Experimental
- Put in the flask: 28g dried salicylic acid.
- Turn on the magnetic stirrer, add 80ml methanol, stir until dissolved.
- Slowly add 8ml (divided into 4 times, each time 2ml separated 15 minutes)
concentrated sulfuric acid.
- Reflux for 5 hours

*Note
- Salicylic acid is easy to dehumidify, so it must be dried before conducting the
experiment.
- Methanol is poisonous, volatile so it must be done in the fume hood.
- Condensed H2SO4 is prone to burns, used must wear gloves.

====================
Experiment 5

PURIFICATION OF METHYL SALICYLATE

Objectives:
- Refine methyl salicylate by methods of extraction, neutralization, drying...
1. Formula and applications
- IUPAC Name: Methyl 2-hydroxybenzoate
- Molecular formula: C8H8O3
- Molecular weight: 152.1494 g/mol
- Structure:

*Application: Methyl salicylate has an analgesic, anti-inflammatory effect, often used in

pain relief patches, pain relief gels...
* Product standards:
- Odorless or yellowish liquid, long-lost black aroma, almost insoluble in water, dissolved in
alcohol, ether. For the purple color with reagents FeCl3
- Density 1,178 - 1,186. Boiling point 219-224C, the refractive index at 20C: 1.535 – 1.530
2. Theoretical basis
- Step1: Remove the impurity by extracting
- Step 2: Neutralizing organic phase to pH=6-7
- Step 4: Re-extract with water
- Step 5: Make anhydrous organic phase
- Step 6: Evaluate the results.
3. Materials and tools
a. Materials used

Material Origin Quantity

NaHCO3 10% China -
Na2SO4 khan China -
b. Tools
Tool Size Amount Tool Amount
Round flask 250ml 1 Electric stove 1
Separating funnel 250ml 1 Small beaker 1
Beaker 100ml 1 Glass rod 1

4. Experimental
- After reflux for 5 hours, cool and extract with 100ml distilled water.
- The oil layer is washed 3 times x 20ml of distilled water.
- Neutralize with NaHCO3 10% to the end of pH = 6 - 7, the oil layer is washed with
20ml distilled water.
- Make anhydrous with Na2SO4.
- Evaluate the results.

*Note
- Na2SO4 had to make anhydrous before use
- Be careful to avoid losing finished product.

====================
Experiment 6
SYNTHESIS OF DIETYPHTALAT

Objectives:
- Preparation dietylphtalate from anhydrite phthalic, ethanol, and sulfuric acid
1. Formula and applications
- IUPAC Name: Diethyl benzene-1,2-dicarboxylate
- Molecular formula: C12H14O4
- Molecular weight: 222.2372 g/mol
- Structure:

*Application: Dietylphtalat has the effect of curing scabies, skin fungus ...
* Product standards:
- Liquid, transparent, colorless or slightly yellow ivory, comparable to oil, has a slight aroma.
- d 420 = 1,123 - 1,125. The boiling point 295C. Almost insoluble in water, easy to dissolve in
alcohol and ether. Dissolve rubber and plastic. Easy to decompose at high temperatures.
2. Theoretical basis
- Perform the esterification reaction
3. Materials and tools
a. Materials used

Material Quantity
Anhydrit phthalic 45g
Ethanol 50ml
Solid sulphuric acid 16ml
b. Tools
Tool Size Amount Tool Amount
Round flask NS29 1 Magnetic stirrer 1
Condenser NS29 1 Electric stove 1
Glass cup 250ml 1 Small beaker 1
Measuring cylinder 25ml 1 Pipet 1
4. Experimental
- Put in the sphere: 45g dried phthalic anhydrite.
- Install the condenser, turn on the magnetic stirrer, add 50 ml of ethanol, stir until
dissolved.
- Slowly add 16ml (divided into 4 times, each time 4 ml 15 minutes apart) concentrated
sulphuric acid.
- Reflux for 4 hours

*Note
- Condensed H2SO4 is prone to burns, when used must wear gloves.
====================
Experiment 7
PURIFICATION OF DIETYPHTALAT

Objectives:
- Purification of dietylphtalate by methods of extraction, neutralization, drying ...
1. Formula and applications
- IUPAC Name: Diethyl benzene-1,2-dicarboxylate
- Molecular formula: C12H14O4
- Molecular weight: 222.2372 g/mol
- Structure:

*Application: Dietylphtalat has the effect of curing scabies, skin fungus ...
* Product standards:
- Liquid, transparent, colorless or slightly yellow ivory, comparable to oil, has a slight aroma.
- d 420 = 1,123 - 1,125. The boiling point: 295C. Almost insoluble in water, easy to dissolve
in alcohol and ether. Dissolve rubber and plastic. Easy to decompose at high temperatures.
2. Theoretical basis
- Step 1: Remove the impurity by extracting
- Step 2: Neutralizing organic phase to pH=8
- Step 3: Re-extract with water to pH 7
- Step 5: Make anhydrous organic phase
- Step 6: Evaluate the results.
3. Materials and tools
a. Materials used

Material Quantity of substances

Na2CO3 -
Na2SO4 anhydrous -
b. Tools
Tool Size Amount Tool Amount
Round flask 250ml 1 Glass rod 1
Separating funnel 250ml 1 Measuring cylinder 1
Glass beaker 250ml 1 Small beaker 1

4. Experimental
- After reflux for 4 hours, let cool to room temperature
- Cool, and extract with 20 ml of distilled water.
- The oil layer is washed 2 times x 20ml of distilled water.
- Neutralized with saturated Na2CO3 until the end of pH = 8, the oil layer is washed
with distilled water to pH=7.
- Make anhydrous with Na2SO4.
- Evaluate the results.

*Note
- Na2SO4 had to make anhydrous before use
- Be careful to avoid losing finished product.
====================
Experiment 8
SYNTHESIS OF ASPIRIN

Objectives:
- Preparation aspirin from axit salixylic, anhydrite axetic and sulfuric acid
- Purification of aspirin by methods of recrystalazation

1. Formula and applications

- IUPAC Name: 2-Acetoxybenzoic acid
- Molecular formula: C9H8O4
- Molecular weight: 180.159 g/mol
- Structure:

*Application: Aspirin is a non-steroidal anti-inflammatory drug that has the effect of

relieving pain, antipyretic, anti-inflammatory, it also has an anti-platelet aggregation effect,
when used in low doses for a long time, it can prevent heart attacks and the formation of clots
in blood vessels
* Product standards:
- White crystalline powder, sour taste, melting point 132 - 1360C.
- Soluble in 300 parts of water, soluble in alcohol, ether, chloroform, alkaline solution, does
not react with FeCl3.
2. Theoretical basis
- Step 1: Carry out O-acylation reaction
- Step 2: Crystallization to collect raw crystals
- Step 3: Purification of raw crystals
- Step 4: Refining
- Step 5: Filtration
- Step 6: Evaluation of results
3. Materials and tools
a. Materials used

Material Property Quantity Mol Notes

Anhydrous salicylic acid 10g
Anhidrit axetic 15ml
Sulphuric acid 98% 2ml

b. Tools
Tool Size Amount Tool Amount
Round flask 250ml 1 Magnetic stirrer 1
Thermometer 0 – 100 C 0
1 Condenser 1
Glass cup 250ml 1 Inox bowl 1
1 Buchner hopper 1

4. Experimental
- Put 10g of anhydrous salicylic acid (dried) in a flask, install reflux condenser, add
15ml acetic anhydrite, add 2ml of concentrated sulfuric acid.
- Heat at 50-600C for 45 minutes.
- Quickly pour the reaction mixture into a glass cup.
- Add 150ml of water, stir vigorously, chill with an external ice, the resulting crystal
is filtered on the Buchner hopper.
- Raw aspirin is dissolved in 30ml of hot alcohol, then pour the solution into 75ml of
hot water.
- Cooling for crystallization, filtering to obtain needle-shaped crystals.
- Dry at 50 – 600C to constant volume.
- Evaluation of results

*Note
- Acetic anhydrite is volatile, when experimenting must be fast and conduct in the fume hood.
- Salicylic acid is easy to absorb moisture, so it must be dried before weighing and carrying
out the reaction.
- Condensed H2SO4 is prone to burns, when used must wear gloves.
====================
Experiment 9
SYNTHESIS OF DIBENZYLIDENEACETONE

Objectives:
- Preparation dibenzylideneacetone from benzaldehyde and acetone
- Purification of dibenzylideneacetone

1. Formula and applications

- IUPAC Name: 1,5-diphenyl-1,4-pentadien-3-one
- Molecular formula: C17H14O
- Molecular weight: 234,29 g/mol
- Structure:

*Application: DBA has the ability to absorb UV rays and protect the skin from sun damage.
Moreover, DBA does not irritate the skin. Therefore, DBA is commonly used in sunscreen
products. Dibenzylideneacetone is also used as a component in sunscreens and as
a ligand in organometallic chemistry.
* Product standards:
- It is a pale-yellow solid insoluble in water, well soluble in n-hexane, toluene, benzene and
moderately soluble in ethanol, melting point 111 - 1130C.
2. Theoretical basis
The trans, trans isomer can be prepared in high yield and purity
by condensation of benzaldehyde and acetone with sodium hydroxide in a water/ethanol
medium followed by recrystallization.
3. Materials and tools
a. Materials used

Material Property Quantity Mol Notes

Acetone 1.3ml
Benzaldehyde 3.6ml
Ethanol 28ml
NaOH (solid) 3.5g
b. Tools
Tool Size Amount Tool Amount
Becher 250ml 1 Magnetic stirrer 1
Becher 50ml 1 Stirring chopsticks 1
Erlen 150ml 1 Pipet 5ml 1
Erlen 250ml 1 Buchner hopper 1
Themomerter 1-1000C 1 Thermostat tank 1

4. Experimental
- Dissolve 3.5 g of NaOH in erlene (250 ml) with 35 ml of water and 28 ml of ethanol.
Stir well and stabilize the temperature between 20°C and 25°C.
- Mix 3.6 ml (0.035 mol) of benzaldehyde and 1.3 ml (0.0175 mol) of acetone in a 50
ml becher, shaking lightly to dissolve. Add half of this mixture to the NaOH solution. Stir
well and stabilize the temperature between 20°C and 25°C. After 15 minutes of reaction, add
the rest to the erlen (re-coat the becher with about 5 ml of alcohol) and continue to let the
reaction occur for another 30 minutes (the same above temperature range).
- Cool the erlen in an ice bath for about 15 minutes and then filter under low pressure.
Disperse the product in 200 ml of water, stir thoroughly, then filter under low pressure, wash
the raw product with water.
- Put the raw DBA in the erlen (150 ml), add about 20 ml of alcohol (at boiling
temperature) and put it on the thermostat tank, shake the erlen well. Continue to add alcohol
slowly (at boiling temperature) until the DBA has completely melted. Cool to room
temperature and then cool in an ice cube. Filter under low pressure, wash DBA with a little
cold alcohol
*Note
- Acetic anhydrite is volatile, when experimenting must be fast and conduct in the fume hood.
- Salicylic acid is easy to absorb moisture, so it must be dried before weighing and carrying
out the reaction.
- Condensed H2SO4 is prone to burns, when used must wear gloves.
====================
Experiment 10

SYNTHESIS OF QUERCETIN

Objectives:
- Synthesis of quercetin from rutin, ethanol, and hydrochloric acid
1. Formula and applications
- IUPAC Name: 2-(3,4-dihydroxyphenyl)-3,5,7-trihydroxy-4H-chromen-4-one
- Molecular formula: C15H10O7
- Molecular weight: 302,236 g/mol
- Structure:

*Application: Quercetin is a plant flavonol from the flavonoid group of polyphenols. It is

found in many fruits, vegetables, leaves, seeds, and grains; capers, red onions, and kale are
common foods containing appreciable amounts of it. It has a bitter flavor and is used as an
ingredient in dietary supplements, beverages, and foods.
* Product standards:
- Yellow crystalline powder, Practically insoluble in water; soluble in aqueous alkaline
solutions
- Density 1.799 g/cm3. Melting point 316C
2. Theoretical basis
- Hydrolysis reaction
3. Materials and tools
a. Materials used

Material Origin Quantity

HCl 36,5% China 10ml
Ethanol China 50ml
Rutin VN 2g
b. Tools
Tool Size Amount Tool Amount
NS29 flask 250ml 1 Magnetic stirrer 1
Separating funnel 250ml 1 Electric stove 1
Condenser NS29 1 Small beaker 1
Themomerter 1-1000C 1 Buchner hopper 1

4. Experimental
- Weigh 2.0g of raw rutin into a 250ml beaker and then dissolve it in 50ml of hot
ethanol.
- Pour the solution into the 3-neck vessel and then proceed to install the reflux
condenser.
- Turn on heating magnetic stirrer.
- Using a drip funnel, slowly drip 10 ml of concentrated HCl acid into the solution.
The reaction is heated at a temperature of 80°C for 2 hours.
- Pour the mixture from the flask into a 100 ml beaker.
- Allow to cool 0-5oC for the mixture to crystallize slowly.
- Carry out filtration of the product collection on the Buchner hopper and wash the
crystals with cold distilled water.
- Qualitative test of quercetin by thin-layer chromatography with a solvent system
deployed as:n-butanol/water/acetic acid = 4:5:1

*Note

- Condensed HCl is volatile so it must be done in the fume hood.

====================
Experiment 11
SYNTHESIS OF P-NITROZOPHENOL

Objectives:
- Synthesis of p-nitrozophenol from phenol, sodium nitrite and sulfuric acid as intermediate
material for the synthesis of p-aminophenol
1. Formula and applications
- IUPAC Name: 4-nitrozophenol
- Molecular formula: C6H5NO2
- Molecular weight: 123,110 g/mole
- Structure:

*Application: Making p-aminophenol preparation raw materials

* Product standards:
- Brown crystals, melting point 156-158C (decomposition).
2. Theoretical basis
- Step 1: Conduct nitrozoization reaction
- Step 2: Filter the precipitate
- Step 3: Wash the precipitate with cold water to pH=4-5
- Step 4: Dry to a constant weight
- Step 6: Evaluate the results.
3. Raw materials and tools
a. Materials used

Material Origin Quantity

Phenol China 50ml
Sodium nitrite China 50g
Sulphuric acid 22% Self-mixing 300ml
Chilling ice - 240g
b. Tools
Tool Size Amount Tool Amount
Round flask 250ml 1 Condenser 1
Separating funnel 250ml 1 Electric stove 1
Glass beaker 250ml 1 Small beaker 1
Measuring cylinder 100ml 1 Buchner funnel 1
pH test paper 1 Glass rod 1

4. Experimental
- Put in a glass beaker 100ml distilled water, 50ml phenol, stir thoroughly for phenol
to diffuse evenly into the water.
- While stirring, add 240g of crushed ice, cool outside, continue stirring for 10 minutes.
- Add 50g sodium nitrite, stir well, and drip slowly 170ml 22% sulphuric acid solution.
Keep the temperature in the flask below 10C.
- Finish dripping, stir for another 15 minutes and then filter the precipitate through the
Buchner funnel.
- Rinse the precipitate to pH= 4-5 (3 times, 30ml each) obtaining brown p-nitrozo-
phenol.
- Evaluate the results

*Note
- Phenols made in fume hood
- Concentrated H2SO4 is easy to burns when used must wear gloves and when diluted
must slowly drop acid into the water and cool outside.

====================
Experiment 12
SYNTHESIS OF P-AMINOPHENOL

Objectives:
- Synthesis of p-aminophenol from p-nitrozophenol, sulfur, NaOH as intermediate materials
for the synthesis of paracetamol
1. Formula and applications
- Name IUPAC: 4-aminophenol
- Molecular formula: C6H7NO
- Molecular weight: 109,128 g/mol
-Structure:

*Application: Intermediate materials for the synthesis of paracetamol

* Finished product standards:
- Black-brown crystals, melting point at 180-182C (sublimation decomposition)
2. Theoretical basis
- Step 1: Preparation Na2S, a reduction agent
- Step 2: Conduct the reduction reaction
- Step 3: Neutralize to pH=7
- Step 4: Filter and wash crystals
- Step 5: Evaluate the results.
3. Raw materials and tools
a. Materials used

Material Origin Quantity

p-nitrozophenol - -
Sulphuric acid 10% Self-mixing -
Chilling ice - 240g
Sulfur powder China 28g
Solid NaOH China 60g
b. Tools
Tools Size Amount Tool Amount
Measuring cylinder 100ml 1 Buchner funnel 1
Thermometer 0 – 1000C 1 Stainless Steel Bowl 1
Beaker 500ml 2 Glass rod 1
Separating funny 250ml 1 pH Test paper -

5. Experimental
- Put in a beaker 500ml: 130ml distilled water and 60g solid NaOH, stir to dissolve.
- Add 28g of powdered sulfur and heat to dissolve completely and then boil for another 40
minutes to obtain Na2S solution (maintain the solution volume of about 150-170ml).
- Lower the temperature to 55-60C, slowly add a little of p-nitrozophenol, maintain the
reaction temperature in the range of 55-65C. Continue stirring and keep at a temperature of
55-65C for another 15 minutes.
- Cool the reactive mixture to a temperature of 5-10C, using a 22% H2SO4 solution to
neutralize to pH= 8-9. Then use sulphuric acid 10% to neutralize to pH = 7 and then leave
the mixture alone for about 1-2 hours.
- Filter the reaction mixture through the Buchner funnel. Rinse with cold water (3 times, 30ml
each time). Draining the water for the last time obtained a black-brown p-amino phenol.
- Evaluate the results

*Note
- Concentrated H2SO4 is easy to burns when used must wear gloves, and when diluted
must slowly drop acid into the water and cool outside.

====================
Experiment 13
SYNTHESIS OF PARACETAMOL
Objectives:
- Synthesis of paracetamol from p-aminophenol, anhydrite acetic
1. Formula and applications
- IUPAC Name: N-(4-hydroxyphenyl) ethanamide
- Molecular formula: C8H9NO2
- Molecular weight: 151,163 g/mol
- Structure:

*Application: Paracetamol is an active ingredient that reduces fever, reduces pain, often used
to prepare tablets, capsules, powdered medicines, mixtures ...
* Product standards:
- The powder or the crystals is white or slightly pink.
- Odorless, melting point: 169 - 172C.
- Dissolved in 70 parts of waters at 80C, dissolved in 7 parts of boiling water or alcohol 95,
in 40 parts of glycerin, in 15 parts of acetone, easy to dissolve in alcohol solution, insoluble
in ether.
2. Theoretical basis
- Step 1: Conduct the N-acylation reaction
- Step 2: Crystallization collect crystals
- Step 3: Filter raw crystals
- Step 4: Refine
- Step 5: Filter, attract crystals
- Step 6: Evaluate the results.
3. Raw materials and tools
a. Materials used

Material Origin Quantity

p-aminophenol - -
Anhydrite acetic China 45ml
Activated carbon China 4g
b. Tools
Tool Size Amount Tool Amount
Round flask 500 ml 1 Electric stove 1
Thermometer 0 – 1000C 1 Buchner funnel 1
Beaker 500ml 2 Inox Bowl 1

5. Experimental
- Put in the flask: p-aminophenol, heat in the water bath to 50-55C, and then add 45ml acetic
anhydrite.
- Continue to simmer this mixture for another 30 minutes. Cool for crystallization. The
mixture contains crystals that are left to cool overnight.
- Filter on the Buchner funnel to run out of acetic acid.
- The resulting raw crystals crystallize with 4 parts of boiled water and 4g of activated carbon.
Boil the mixture for 30-40 minutes to bleach the color 1st time, hot quickly filter.
- Filter fluid is bleached for the second time with activated carbon, hot quickly filter
- To precipitate to collect pink-white paracetamol crystals.
- Evaluate the results

*Note
- Anhydride acetic causes eye irritation, so when used must be made in the fume hood

====================