Thionyl Chloride → 2,4,5-Trifluoro-3-difluoromethoxybenzoyl chloride

HRID 1440094노트

반응식

HRID 1440094 반응식
S(Cl)([Cl:3])=O.[F:5][CH:6]([F:20])[O:7][C:8]1[C:9]([F:19])=[C:10]([CH:14]=[C:15]([F:18])[C:16]=1[F:17])[C:11](O)=[O:12]>C1C=CC=CC=1>[F:5][CH:6]([F:20])[O:7][C:8]1[C:9]([F:19])=[C:10]([CH:14]=[C:15]([F:18])[C:16]=1[F:17])[C:11]([Cl:3])=[O:12]

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 150237813-(Difluoromethoxy)-2,4,5-trifluorobenzoic acid

생성물 1

HCID 152829712,4,5-Trifluoro-3-difluoromethoxybenzoyl chloride

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

15 ml of thionyl chloride were added to a solution of 5.22 g (0.0216 moles) of 3-difluoromethoxy-2,4,5-trifluorobenzoic acid [(XII), R1 --OCHF2, R3' =H, X=X'=F] (prepared as described in Preparation 1, 2 or 3) in 300 ml of benzene, and the mixture was heated under reflux for 3 hours. At the end of this time, benzene and excess thionyl chloride were removed by distillation under reduced pressure, to give 3-difluoromethoxy-2,4,5-trifluorobenzoyl chloride [(XIII), R1 =--OCHF2, R3' =H, X=X'=F].

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 3 hours
  3. customAt the end of this time, benzene and excess thionyl chloride were removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-b0ff91b097ed40f2a0570db0ed63a639
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05496951

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