반응 #416403

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ethyl chloride

triethyl phosphite

acetyl chloride

Ethyl chloride

→

diethyl acetylphosphonate

수율 98.0%

반응 조건

후처리

1. 1
   온도maintained
2. 2
   온도by cooling
3. 3
   workup.DISTILLATIONThe product was distilled under vacuum

실험 절차

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.

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