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Acetyl chloride → 2'-Chloro-4',5'-difluoroacetophenone

HRID 974658
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HRID 974658 반응식
[C:1](Cl)(=[O:3])[CH3:2].[Cl:5][C:6]1[CH:11]=[CH:10][C:9]([F:12])=[C:8]([F:13])[CH:7]=1.[Cl-].[Al+3].[Cl-].[Cl-]>>[CH3:2][C:1]([C:11]1[C:6]([Cl:5])=[CH:7][C:8]([F:13])=[C:9]([F:12])[CH:10]=1)=[O:3]
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참가 물질

4

반응물 3

HCID 6367Acetyl chlorideHCID 1365194-Chloro-1,2-difluorobenzeneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 27364892'-Chloro-4',5'-difluoroacetophenone수율 82%

반응 조건

온도
120 °C

실험 절차

23.6 g (0.3 mol) of acetyl chloride was added to a mixture comprising 29.7 g (0.2 mol) of 1-chloro-3,4-difluorobenzene and 40.0 g (0.3 mol) of aluminum chloride at a temperature of from 20° to 40° C. Then, the mixture was stirred at 120° C. for two hours. While still being hot, the mixture was poured on 250 g of ice, and the separated oil was extracted with ethylene chloride. The extract was neutralized and washed with water, and the solvent was distilled off under reduced pressure to obtain 31.2 g (yield: 82%) of 2-chloro-4,5-difluoroacetophenone. This compound was analyzed, and the analytical values were as follows.

후처리

  1. extractionthe separated oil was extracted with ethylene chloride
  2. washwashed with water
  3. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-659cd691d1974f5183cd1cf7e269c820
출처 데이터셋
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05068449

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