Chlorosulfonic acid → 2,4-Difluoro-3-methylbenzenesulfonyl chloride

HRID 337815노트

반응식

HRID 337815 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[CH3:9].[S:10]([Cl:14])(=O)(=[O:12])[OH:11]>O>[F:1][C:2]1[C:3]([CH3:9])=[C:4]([F:8])[CH:5]=[CH:6][C:7]=1[S:10]([Cl:14])(=[O:12])=[O:11]

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 5814931,3-Difluoro-2-methylbenzene

생성물 1

HCID 157253752,4-Difluoro-3-methylbenzenesulfonyl chloride수율 98%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 1,3-difluoro-2-methylbenzene (5.00 g, 39.0 mmol), chlorosulfuric acid (10.5 mL, 158 mmol) was added with cooling on ice, and the mixture was stirred at room temperature for 5 hours. To the reaction solution, water (100 mL) was added with cooling on ice, followed by extraction with dichloromethane (100 mL). The thus obtained organic layer was dried over anhydrous sodium sulfate. After vacuum concentration, the residue was purified with silica gel chromatography to yield the title compound (8.65 g, 98%) as a colorless amorphous solid.

후처리

  1. temperaturewith cooling on ice
  2. temperaturewith cooling on ice
  3. extractionfollowed by extraction with dichloromethane (100 mL)
  4. dry with materialThe thus obtained organic layer was dried over anhydrous sodium sulfate
  5. concentrationAfter vacuum concentration
  6. customthe residue was purified with silica gel chromatography

출처 및 근거

ORD 기록
ord-897fe641414d4a7faf9fbd47220992ae
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889741B2

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