Object:
Preparation of benzilic acid in benzil.
(I) Preparation of Benzil step I
Chemical Required:
Benzoin
- 10
gm
Acetic
acid - 50ml
Conc.
HNO3 - 25ml
Procedure:
A
mixture of benzoin (10gm, 0.047 mole), acetic acid (50 ml) and concentrated HNO3
(25ml) is heated in a round bottom flask boiling water bath for 2hrs. The
flask is connected to a trap containing NaOH solution to absorb oxides of
nitrogen. Alternatively, the reaction is carried out in a fume cupboard. The
reaction mixture is cooled, poured with stirring into an ice cold water. The
mixture is stirred well and the separated product filtered and wash with water.
It is crystallized from rectified spirit
as yellow prisms.
yield – 8.7
mpt
- 95°C
Second step-
Preparation of benzilic acid from benzil
Chemical Required-
Benzil
– 8 gm
Potassium
Hydroxide pellets – 10 gm (in 20ml H2O)
Rectified
spirit – 25 ml
Conc.
HCl – 35 ml
A
mixture of benzil (8 gm 0.038 mole), KOH solution (10 gm dissolved is 20ml
water) and rectified spirit (25ml) is refluxed in water bath for 12 minutes.
The hot reaction mixture is poured into water (150 ml) contained in a beaker.
In case the reaction does not go to completion a colloidal solution is obtained
due to separation of unreacted benzil.
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