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Ethyl fluoroacetate → 1-(5-Bromo-2-fluorophenyl)-2-fluoroethanone

HRID 930274
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HRID 930274 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[C:4](I)[CH:3]=1.[Li]CCCC.[F:15][CH2:16][C:17](OCC)=[O:18]>C1COCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[C:4]([C:17](=[O:18])[CH2:16][F:15])[CH:3]=1
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참가 물질

5

반응물 3

HCID 9988Ethyl fluoroacetateHCID 27827504-Bromo-1-fluoro-2-iodobenzeneHCID 178418339Butyllithium

생성물 1

HCID 867157171-(5-Bromo-2-fluorophenyl)-2-fluoroethanone수율 63%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-78 °C

실험 절차

A solution of 4-bromo-1-fluoro-2-iodobenzene (5.0 g, 116 mmol, (1), Aldrich) in THF (60 ml) under nitrogen atmosphere was cooled to −78° C. A solution of n-BuLi (2.5M in hexanes; 7.31 ml, 18.28 mmol, Aldrich) was added drop wise and the reaction was stirred at −78° C. for one hour. Ethyl monofluoroacetate (2.1 g, 19.94 mmol, Aldrich) was added drop wise and the reaction was stirred at −78° C. for one hour. The reaction was quenched with aqueous saturated ammonium chloride solution and allowed to warm to RT. The reaction was diluted with water and EtOAc. The organic layer was separated, washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. The material was purified via silica gel flash chromatography using a gradient of 0-20% EtOAc in Hexanes to afford the title compound as an off white solid. (2.45 g, 10.42 mmol, 63% yield). MS m/z=234.9 M+. Calculated for C8H5BrF2O: 235.03

후처리

  1. stirringthe reaction was stirred at −78° C. for one hour
  2. customThe reaction was quenched with aqueous saturated ammonium chloride solution
  3. temperatureto warm to RT
  4. additionThe reaction was diluted with water and EtOAc
  5. customThe organic layer was separated
  6. washwashed with brine
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe material was purified via silica gel flash chromatography

출처 및 근거

ORD 기록
ord-f31efca221ea4359a3a43617e7784d7f
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296734B2

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