反应详情

温度

10 °C

A 40.3 g. portion of sodium amide was suspended in 400 ml. of dry toluene at 70° C. and 199.6 g. of diphenylacetonitrile, dissolved in 600 ml. of hot dry toluene, was added dropwise. The mixture was stirred at 70°-100° C. for 4 hours, and an additional 500 ml. of dry toluene and 100 ml. of dimethylformamide were added. The mixture was stirred for 27 hours more. The slurry was cooled to 10° C., and 114.6 g. of 2,3-dichloropropene was added. The mixture was warmed to ambient temperature and stirred for 40 hours, and was then stirred at 90°100° C. for one hour. The mixture was then cooled to ambient temperature, diluted with a large amount of diethyl ether, washed with water and dried over magnesium sulfate. The solution was evaporated to give 265 g. of crude liquid product.

1. customat 70° C.
2. stirringThe mixture was stirred for 27 hours more
3. temperatureThe mixture was warmed to ambient temperature
4. stirringstirred for 40 hours
5. stirringwas then stirred at 90°100° C. for one hour
6. temperatureThe mixture was then cooled to ambient temperature
7. washwashed with water
8. dry with materialdried over magnesium sulfate
9. customThe solution was evaporated
10. customto give 265 g