Chloroethane → Diethyl acetylphosphonate

HRID 325260

반응식

[P:1]([O:9][CH2:10][CH3:11])([O:6][CH2:7][CH3:8])([O:3]CC)=O.[C:12](Cl)(=[O:14])[CH3:13].C(Cl)C>>[C:12]([P:1](=[O:3])([O:6][CH2:7][CH3:8])[O:9][CH2:10][CH3:11])(=[O:14])[CH3:13]

참가 물질

반응물 3

HCID 6337Chloroethane2회

HCID 6367Acetyl chloride

HCID 6535Triethyl Phosphate

생성물 1

HCID 522997Diethyl acetylphosphonate수율 98%

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.

후처리

temperaturemaintained
temperatureby cooling
distillationThe product was distilled under vaccum

출처 및 근거

ORD 기록: ord-e23e4fc29f8149ea9d146b841f182704
출처 데이터셋: uspto-grants-1984_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04440646

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