Cyclohex-1-en-1-ylphosphonic acid → Cyclohexene-1-phosphonic acid dichloride

반응식

C1(P(O)(=O)O)CCCCC=1.C(Cl)(Cl)=O.[C:15]1([P:21]([Cl:24])([Cl:23])=[O:22])[CH2:20][CH2:19][CH2:18][CH2:17][CH:16]=1>>[C:15]1([P:21]([Cl:24])([Cl:23])=[O:22])[CH2:20][CH2:19][CH2:18][CH2:17][CH:16]=1

참가 물질

반응물 2

HCID 14979139Cyclohex-1-en-1-ylphosphonic acid

HCID 88837489HCID 88837489, 화합물

생성물 1

HCID 23415522Cyclohexene-1-phosphonic acid dichloride수율 928.2%

실험 절차

Into a mixture of 57 g of cyclohexene-1-phosphonic acid and 10 g of cyclohexene-1-phosphonic acid dichloride phosgene was introduced at a temperature of from 170°-180°C for 19 hours. At the end of the reaction, nitrogen was blown through the mixture to remove excess phosgene and subsequently the mixture was distilled under reduced pressure. 62 g of cyclohexene-1-phosphonic acid dichloride were obtained, b.p. 75°C under 0.3 mm Hg, corresponding to a yield of 89.5 percent of the theory.

후처리

additionwas introduced at a temperature of from 170°-180°C for 19 hours
customAt the end of the reaction, nitrogen
customto remove excess phosgene
distillationsubsequently the mixture was distilled under reduced pressure

출처 및 근거

ORD 기록: ord-4d5e81281786499780c91e68c69c95b8
출처 데이터셋: uspto-grants-1976_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US03950413

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