Chloroethane → Diethyl acetylphosphonate

HRID 329221

반응식

[P:1]([O:8][CH2:9][CH3:10])([O:5][CH2:6][CH3:7])[O:2]CC.[C:11](Cl)(=[O:13])[CH3:12].C(Cl)C>>[C:11]([P:1](=[O:2])([O:5][CH2:6][CH3:7])[O:8][CH2:9][CH3:10])(=[O:13])[CH3:12]

참가 물질

반응물 3

HCID 6337Chloroethane2회

HCID 6367Acetyl chloride

HCID 31215Triethyl phosphite

생성물 1

HCID 522997Diethyl acetylphosphonate수율 98%

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.

후처리

temperaturemaintained
temperatureby cooling
distillationThe product was distilled under vacuum

출처 및 근거

ORD 기록: ord-2dd7db1a4f0143b89435b1782c08c5c9
출처 데이터셋: uspto-grants-1977_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04020091

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