- Production Method of Benzoin acetate
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acetate (CAS NO.: ) could be produced through the following synthetic routes.
To a mixture of 212 g. (1 mole) of benzoin, 200 cc. of glacial acetic acid, and 200 cc. (2.1 moles) of acetic anhydride, in a 1-l. beaker provided with a mechanical stirrer, is added slowly, with stirring, 20 cc. of concentrated c.p. sulfuric acid. This requires five minutes, during which the benzoin quickly dissolves and the temperature rises to about 50°. The beaker is placed on the steam bath for twenty minutes. The mixture is allowed to cool somewhat, transferred to a large dropping funnel, and added slowly to 2.5 l. of water vigorously stirred in a 4-l. (1-gal.) crock during thirty minutes. Stirring is continued for one hour. The mixture is filtered by suction on a 30-cm. Büchner funnel, and the crystals are sucked as dry as possible and spread on filter paper. After about two hours the crystals are transferred to a 1-l. beaker and warmed to about 60° with 400 cc. of 95 per cent ethyl alcohol. The clear solution is cooled with stirring to 5° and filtered by suction. The air-dried benzoin acetate, melting at 80–82°, weighs 220–230 g. (86 to 90 per cent of the theoretical amount). Another crystallization from 400 cc. of alcohol removes the slight yellow tinge and gives a product melting at 81.5–82.5°, with a loss of about 10 g.
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