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

HRID 34071ノート

反応式

HRID 34071 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f574309933cb4930a12807a587ce64b2
出典データセット
uspto-grants-2008_09
特許番号
US07429609B2

反応ノート

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