反应详情

168.18 g (1.0 mole) of benzil in 2 liters of ethyl ether was placed in a 5 liter, three necked round bottomed flask, fitted with a reflux condenser, mechanical stirrer, addition funnel and nitrogen bypass. All of the glassware was flame-dried before use while being flushed with nitrogen. A 3 molar solution in ethyl ether of phenyl magnesium bromide (181.23 g, 1.0 mole) was then placed in the addition funnel and added dropwise to the flask over a period of 1.5 hours. The solution was then refluxed overnight. Hydrolysis of the Grignard complex was then accomplished using a 10% solution of H2SO4 with the concurrent addition of 1.5 liters of CHCl3. After complete hydrolysis, the organic layer was separated and washed with one liter of water. The organic layer was dried with magnesium sulfate, concentrated and recrystallized with hexane to give phenylbenzoin (m.p. 87°-88°, lit 88° C.) of 99% purity in yield of 62%.

1. customfitted with a reflux condenser, mechanical stirrer, addition funnel
2. customAll of the glassware was flame-dried before use
3. customwhile being flushed with nitrogen
4. additionadded dropwise to the flask over a period of 1.5 hours
5. temperatureThe solution was then refluxed overnight
6. customHydrolysis of the Grignard complex
7. customAfter complete hydrolysis
8. customthe organic layer was separated
9. washwashed with one liter of water
10. dry with materialThe organic layer was dried with magnesium sulfate
11. concentrationconcentrated
12. customrecrystallized with hexane