Sodium Thiosulfate → (5-Bromo-2-chlorothiophen-3-yl)methanol

HRID 34071노트

반응식

HRID 34071 반응식
[Cl:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[CH2:7][OH:8].[Br:9]N1C(=O)CCC1=O.S([O-])([O-])(=O)=S.[Na+].[Na+]>CN(C)C=O.C(OCC)(=O)C>[Br:9][C:4]1[S:3][C:2]([Cl:1])=[C:6]([CH2:7][OH:8])[CH:5]=1

참가 물질

6

반응물 3

HCID 24477Sodium ThiosulfateHCID 67184N-bromobutanimideHCID 18938072(2-Chlorothiophen-3-yl)methanol

생성물 1

HCID 23070160(5-Bromo-2-chlorothiophen-3-yl)methanol수율 80.6%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 3.0 g of (2-chlorothiophen-3-yl)methanol in 60 mL of dimethylformamide was added 3.59 g of N-bromosuccinimide at room temperature, and stirred at this temperature for 2 hours. Adding 10 mL of 10% sodium thiosulfate, and the resultant solution was diluted with ethyl acetate. The organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated, to afford 3.7 g of the title compound as a colorless oil.

후처리

  1. washThe organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-f574309933cb4930a12807a587ce64b2
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429609B2

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