반응 #412442

ord-e23e4fc29f8149ea9d146b841f182704

반응 방정식

CCCl
ethyl chloride
CCOP(=O)(OCC)OCC
triethyl phosphate
CC(=O)Cl
acetyl chloride
CCCl
Ethyl chloride
CCOP(=O)(OCC)C(C)=O
diethyl acetylphosphonate
수율 98.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

166.2 grams (1 mole) triethyl phosphate 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 vaccum 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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04440646uspto-grants-1984_04