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1-(4-Bromo-2-thienyl)ethan-1-one → 2-Bromo-1-(4-bromo-2-thienyl)ethanone

HRID 470199
ノート
印刷プレビュー

反応式

HRID 470199 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:7](=[O:9])[CH3:8])[S:5][CH:6]=1.[Br-:10].[Br-].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC>CO.ClCCl>[Br:10][CH2:8][C:7]([C:4]1[S:5][CH:6]=[C:2]([Br:1])[CH:3]=1)=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 27352371-(4-Bromo-2-thienyl)ethan-1-oneHCID 23500184Tetra-n-butylammonium tribromide

生成物 1

HCID 128903462-Bromo-1-(4-bromo-2-thienyl)ethanone

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

To 1-(4-bromothiophen-2-yl)ethanone (10 g, 48.8 mmol) in methanol (98 mL) and dichloromethane (163 mL) is added tetra-n-butylammonium tribromide (28.8 g, 58.5 mmol). The reaction mixture is concentrated under reduced pressure at 50° C. to give a residue which is purified by silica gel chromatography, eluting with dichloromethane to give crude 2-bromo-1-(4-bromo-2-thienyl)ethanone. To a solution of the crude 2-bromo-1-(4-bromo-2-thienyl)ethanone in acetonitrile (200 ml) is added potassium carbonate (20.2 g, 146 mmol) and diallylamine (9.48 g, 97.5 mmol). The reaction is stirred at room temperature for 2 hours. Water is added and the solution is extracted with ethyl acetate. The organic phases are combined, dried over sodium sulfate, filtered, and concentrated under reduced pressure to give the crude title compound. ES/MS (m/e): (79Br/81Br) 300/302 (M+H).

後処理

  1. concentrationThe reaction mixture is concentrated under reduced pressure at 50° C.
  2. customto give a residue which
  3. customis purified by silica gel chromatography
  4. washeluting with dichloromethane

出典と根拠

ORDレコード
ord-2b94a2d7c301424e84e71d0807e94e82
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629270B2

反応ノート

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