Water → 4-[(4-Chlorobenzyl)sulfonyl]-1,2-difluorobenzene

HRID 1686428ノート

反応式

HRID 1686428 の反応式
[F:1][C:2]1[CH:3]=[C:4]([SH:9])[CH:5]=[CH:6][C:7]=1[F:8].Br[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=1.C(=O)([O-])[O-:20].[K+].[K+].[OH2:25]>CN(C=O)C>[Cl:18][C:15]1[CH:16]=[CH:17][C:12]([CH2:11][S:9]([C:4]2[CH:5]=[CH:6][C:7]([F:8])=[C:2]([F:1])[CH:3]=2)(=[O:20])=[O:25])=[CH:13][CH:14]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 693291-(Bromomethyl)-4-chlorobenzeneHCID 27783783,4-Difluorobenzenethiol

生成物 1

HCID 689551304-[(4-Chlorobenzyl)sulfonyl]-1,2-difluorobenzene

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3,4-difluorobenzenethiol (1.0 g), 1-(bromomethyl)-4-chlorobenzene (1.28 g) and potassium carbonate (0.94 g) in DMF (10 ml) was stirred overnight at RT then diluted with water, extracted with ether, and the organics dried (MgSO4) and evaporated under reduced pressure. The resulting oil was dissolved in DCM (10 ml) and MCPBA (2.94 g) added and stirred at RT overnight. The solution was then washed with aqueous sodium metabisulphite and aqueous sodium hydrogen carbonate, dried (MgSO4) and evaporated under reduced pressure to give a solid, triturated with isohexane to give the subtitle compound as a white solid (2.3 g).

後処理

  1. extractionextracted with ether
  2. dry with materialthe organics dried (MgSO4)
  3. customevaporated under reduced pressure
  4. dissolutionThe resulting oil was dissolved in DCM (10 ml)
  5. additionMCPBA (2.94 g) added
  6. washThe solution was then washed with aqueous sodium metabisulphite and aqueous sodium hydrogen carbonate
  7. dry with materialdried (MgSO4)
  8. customevaporated under reduced pressure
  9. customto give a solid
  10. customtriturated with isohexane

出典と根拠

ORDレコード
ord-be0ac17b18fe42e5ad79018a15ea30a6
出典データセット
uspto-grants-2012_04
特許番号
US08148572B2

反応ノート

読み込み中…