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

HRID 337815ノート

反応式

HRID 337815 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 157253752,4-Difluoro-3-methylbenzenesulfonyl chloride収率 98%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-897fe641414d4a7faf9fbd47220992ae
出典データセット
uspto-grants-2014_11
特許番号
US08889741B2

反応ノート

読み込み中…