反应详情

To a two-liter-round-bottomed flask fitted with an overhead stirrer, addition funnel and a condenser was added 400 ml of acetone and 85.0 g (1.12 moles) of ammonium thiocyanate. To this solution was added 140.6 g (1.00 moles) of benzoyl chloride. The resultant slurry was heated at reflux for 15 minutes and then the heat was removed and 200 ml of concentrated ammonium hydroxide was added at a rate to maintain reflux. The reaction mixture was heated at reflux for an additional 15 minutes and then cooled to room temperature. This mixture was added to 6 liters of water, and the resulting precipitate was collected by filtration and washed with 2 liters of water, then air dried and recrystallized from 1.5 liters of ethanol to give 98.5 g of the desired product as a white solid, mp 170°-171° C.

1. customTo a two-liter-round-bottomed flask fitted with an overhead stirrer, addition funnel and a condenser
2. temperatureThe resultant slurry was heated
3. temperatureat reflux for 15 minutes
4. customthe heat was removed
5. addition200 ml of concentrated ammonium hydroxide was added at a rate
6. temperatureto maintain
7. temperaturereflux
8. temperatureThe reaction mixture was heated
9. temperatureat reflux for an additional 15 minutes
10. additionThis mixture was added to 6 liters of water
11. filtrationthe resulting precipitate was collected by filtration
12. washwashed with 2 liters of water
13. customair dried
14. customrecrystallized from 1.5 liters of ethanol