Benzocaine 1.

Recrystallization of Benzocaine

1. Weighed 5 g of p-aminobenzoic 1. Transferred the crude

acid. benzocaine into a beaker.
2. Dissolved it in 40 mL of 2. Added a minimal amount of
absolute ethanol in a round- hot aqueous ethanol (ethanol +
bottom flask equipped with a water mixture, usually 1:1).
magnetic stir bar. 3. Heated the mixture gently until
3. Cooled the solution in an ice the solid dissolved completely.
bath. 4. If insoluble impurities were
4. Slowly added 1 mL of present, hot filtered the
concentrated sulfuric acid to solution using a preheated
the cold mixture. funnel.
5. Heated the reaction mixture 5. Allowed the filtrate to cool
under gentle reflux for about 7 slowly to room temperature,
minutes. then placed it in an ice bath to
6. Allowed the reaction mixture to complete crystallization.
cool to room temperature. 6. Filtered the purified
7. Transferred the contents to a benzocaine crystals using
beaker containing 30 mL of vacuum filtration.
water. 7. Washed the crystals with a
8. Added sodium bicarbonate small amount of cold water.
solution gradually to neutralize 8. Dried the purified product at
the acid. room temperature.
9. Filtered the resulting
Benzocaine precipitate.
10. Rinsed the solid with cold 🔹 2. Recrystallization of Benzil
water and allowed it to dry.
11. Recrystallized the crude
product from aqueous alcohol
to obtain pure Benzocaine. 1. Placed the crude benzil in a
beaker.
2. Added a small volume of hot
ethanol (or ethyl acetate) to
BENZIL FROM Benzocaine
dissolve the solid.
3. Heated the mixture gently until
the benzil fully dissolved.
1. Dissolve Benzoin (5 g) in 20 mL 4. Filtered the hot solution if
of concentrated nitric acid in a needed to remove insoluble
beaker. impurities.
2. Place the beaker on a water 5. Cooled the solution slowly at
bath and heat gently for about room temperature, followed by
30–45 minutes, occasionally an ice bath.
stirring. 6. Filtered the yellow benzil
3. A yellow crystalline solid crystals.
(benzil) will start to form as the 7. Washed with cold ethanol or
reaction proceeds. water.
4. After completion, cool the 8. Dried the crystals to obtain
mixture in an ice bath to pure benzil.
precipitate out more benzil.
5. Filter the crystals using a
Buchner funnel and wash with
3. Recrystallization of Phenytoin (5,5-
cold water.
6. Recrystallize the crude product Diphenylhydantoin)
from ethanol to obtain pure
benzil.
7. Dry the final product. 1. Transferred the crude
phenytoin to a beaker.
2. Added hot ethanol (or
5,5-DIPHENYL THYDNTAIN FRM BENZIL ethanol:water mixture) in small
amounts to dissolve it.
3. Heated gently while stirring
until fully dissolved.
 Weighed about 5 g of benzil 4. Filtered hot if any insoluble
and transferred it to a round- residue was present.
bottom flask. 5. Cooled the filtrate gradually,
 Added 3 g of urea to the flask. then placed in an ice bath to
 Dissolved the mixture in 25 mL enhance crystal formation.
of ethanol. 6. Filtered the white/pale crystals.
 Added 10 mL of 10% sodium 7. Washed with a little cold
hydroxide (NaOH) solution to ethanol.
the reaction mixture. 8. Dried to obtain pure phenytoin.
 Attached a reflux condenser to
the flask.
 Heated the mixture under 4. Recrystallization of 2,3-
reflux for 30–45 minutes with
constant stirring. Diphenylquinoxaline
 Monitored the reaction until
the solution became
homogeneous and slightly 1. Placed the crude product in a
yellowish. beaker.
 Allowed the reaction mixture to 2. Added hot ethanol (preferred
cool to room temperature. solvent) in small amounts.
 Acidified the mixture carefully 3. Heated until the solid dissolved
using concentrated completely.
hydrochloric acid (HCl) until a 4. Hot filtered if necessary to
white precipitate appeared. remove impurities.
 Filtered the precipitate using 5. Allowed to cool at room
vacuum filtration. temperature, then placed in ice
 Washed the solid with cold bath.
water to remove residual acid 6. Filtered the yellow crystals
and impurities. formed.
 Recrystallized the crude 7. Washed with cold ethanol.
product from ethanol to obtain 8. Dried the final purified 2,3-
pure 5,5-diphenylhydantoin diphenylquinoxaline.

2,3-DIPHENYL QUINOAOXALINE Benzimidazole

1. Weighed approximately 2.1 g  Mixed 27 g o-

of benzil and 1.1 g of o- phenylenediamine with 17.5 g
phenylenediamine. of 90% formic acid in a 250 mL
2. Transferred both solids into a round-bottom flask.
round-bottom flask.  Heated the mixture on a water
3. Added about 25 mL of ethanol bath at 100°C for 2 hours, then
to the flask to dissolve the cooled to room temperature.
reactants.  Added 10% sodium hydroxide
4. Stirred the mixture thoroughly until the solution became
to ensure complete dissolution. alkaline.
5. Heated the solution under  Filtered the precipitated crude
reflux for 30–45 minutes to benzimidazole and washed with
allow condensation. ice-cold water.
6. After completion, cooled the  Dissolved the crude product in
reaction mixture to room 400 mL boiling water, added 2
temperature (or placed in an g activated charcoal, and
ice bath). digested for 15 minutes.
7. Observed the formation of a  Hot-filtered through a Buchner
yellow or pale precipitate funnel, then cooled the filtrate
(product). to 10°C.
8. Filtered the precipitate using  Collected the recrystallized
vacuum filtration. benzimidazole, washed with
9. Washed the solid with cold cold water, and dried at 100°C.
ethanol to remove impurities.
10. Dried the crude product at
room temperature or in a
drying oven.
11. Recrystallized the product
from ethanol to obtain pure
2,3-diphenylquinoxaline.