反应详情

166.2 grams (1 mole) triethyl phosphite was added dropwise with stirring to 78.4 grams (1 mole) of acetyl chloride over a period of 30 minutes at a temperature of 30° to 35° C maintained by cooling. Ethyl chloride was evolved. The temperature was increased to 60° C over the next 1 hour and 15 minutes, at which time the evolution of ethyl chloride was complete. The product was distilled under vacuum yielding 176 grams of diethyl acetylphosphonate (DEAP) in 98% yield, B.P. about 80° C at 5 mm and having a refractive index of 1.4240 at 200° C.

1. temperaturemaintained
2. temperatureby cooling
3. distillationThe product was distilled under vacuum