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

HRID 338071
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HRID 338071 반응식
[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]
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참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-480a16c86cde4487aa6330925aa96a1d
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08889856B2

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