Triphenylphosphine → o-Trifluoromethylbenzyltriphenyl-phosphonium chloride

HRID 904767

반응식

HRID 904767 반응식
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH2:5][Cl:6].[C:13]1([P:19]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C1(C)C(C)=CC=CC=1>[Cl-:6].[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH2:5][P+:19]([C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1)([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 890281-(Chloromethyl)-2-(trifluoromethyl)benzene

생성물 1

HCID 20477565o-Trifluoromethylbenzyltriphenyl-phosphonium chloride

시약·촉매·용매 1

HCID 7237O-Xylene용매

반응 조건

온도
150 °C

실험 절차

214 g (1.1 mols) of o-trifluoromethylbenzyl chloride are initially introduced into the reaction vessel and are heated to about 150° C. A hot solution, at about 100° C., of 262 g (1 mol) of triphenylphosphine in 115 ml of xylene is added thereto, whilst stirring. Stirring is continued at 150° C. for a short time, the mixture is cooled to 20° C. and the crystal sludge is filtered off and washed with cyclohexane/methylene chloride (7:3). After drying at 170° C. and under 0.1 mm Hg, 412 g (90.2% of the theoretical yield) of o-trifluoromethylbenzyltriphenyl-phosphonium chloride are obtained.

후처리

  1. stirringStirring
  2. customis continued at 150° C. for a short time
  3. temperaturethe mixture is cooled to 20° C.
  4. filtrationthe crystal sludge is filtered off
  5. washwashed with cyclohexane/methylene chloride (7:3)
  6. customAfter drying at 170° C. and under 0.1 mm Hg, 412 g (90.2% of the

출처 및 근거

ORD 기록
ord-ef7c27e79cb04f4185665ad69cb4aa1c
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04420225

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