Thionyl Chloride → 1,1'-(Chloromethylene)bis(4-fluorobenzene)

HRID 414485

반응식

HRID 414485 반응식
[F:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6](O)[C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.S(Cl)([Cl:19])=O>O>[F:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6]([Cl:19])[C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 1230494,4'-Difluorobenzhydryl alcohol

생성물 1

HCID 27237731,1'-(Chloromethylene)bis(4-fluorobenzene)수율 88.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 15.0 g (68.1 mmol) of 4,4'-difluorobenzhydrol was added 14.9 ml (204 mmol) of thionyl chloride in the atmosphere of argon, and the mixture was stirred at room temperature for 30 minutes. To the resulting mixture was added water followed by extraction with benzene. The organic layer was successively washed with water, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue thus obtained was subjected to column chromatography on silica gel. There was yielded 14.32 g (60 mmol) of 4,4'-difluorobenzhydryl chloride from the fraction eluted with benzene.

후처리

  1. extractionfollowed by extraction with benzene
  2. washThe organic layer was successively washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue thus obtained

출처 및 근거

ORD 기록
ord-f399839528ef486585527d95483c9819
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04792553

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