反应详情

温度

110 °C

Into a 250 ml round bottomed flask equipped with magnetic stirring and a reflux condenser was placed 15 g (98 mmol) of POCl3, 30 g (145 mmol) of PCl5, and 19.9 g (123 mmol) of α,α-dimethylbenzyl methyl ketone. The reaction was heated in an oil bath to an external temperature of 110° C. Gas evolution ceased after one hour. The reaction was cooled and carefully poured onto ice and aqueous ammonium hydroxide. Extractive workup with diethyl ether gave a mixture of 1-(α,α-dimethylbenzyl)-1-chloroethylene and 1-(α,α-dimethylbenzyl)-1,1-dichloroethane. Vacuum distillation gave purified 1-(α,α-dimethylbenzyl)-1-chloroethylene bp (23 torr) 110-120° C.

1. customInto a 250 ml round bottomed flask equipped
2. customa reflux condenser was placed
3. temperatureThe reaction was cooled
4. distillationVacuum distillation
5. customgave
6. custompurified 1-(α,α-dimethylbenzyl)-1-chloroethylene bp (23 torr) 110-120° C.