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

HRID 414482

반응식

HRID 414482 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 90.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 5.00 g (22.7 mmol) of 4,4'-difluorobenzhydrol was added 16.5 ml (227 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 saturated sodium hydrogen carbonate solution and 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 4.90 g (20.5 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 saturated sodium hydrogen carbonate solution and 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-3105e40af57f46429c343abecd5a1306
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04792553

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