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

HRID 2371572
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HRID 2371572 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%

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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. Boiling point: 65°-67° C./4-5 mmHg.

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-e68ac47e595749d0a8c19185aa219cfb
출처 데이터셋
uspto-grants-1992_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05093515

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