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

HRID 1686428노트

반응식

HRID 1686428 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-be0ac17b18fe42e5ad79018a15ea30a6
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148572B2

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