Ethanol → Ethyl 3-(2-fluorophenyl)prop-2-enoate

HRID 362827

반응식

HRID 362827 반응식
[F:1][C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[CH:4]=[CH:5][C:6]([OH:8])=[O:7].S(Cl)(Cl)=O.[CH2:17](O)[CH3:18]>>[F:1][C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[CH:4]=[CH:5][C:6]([O:8][CH2:17][CH3:18])=[O:7]

참가 물질

4

반응물 3

HCID 702EthanolHCID 24386Thionyl ChlorideHCID 679773-(2-Fluorophenyl)prop-2-enoic acid

생성물 1

HCID 590919Ethyl 3-(2-fluorophenyl)prop-2-enoate수율 96%

실험 절차

A solution of 2-fluorocinnamic acid (48.4 g, 0.29 mol, Aldrich) and thionyl chloride (5 mL) in ethanol (650 mL) was heated to reflux for 48 h. The mixture was concentrated in vacuo. The residue was taken up in ethyl acetate, washed successively with a 5% aqueous sodium bicarbonate solution, water and brine, and dried (Na2SO4). Filtration and concentration gave 54.25 g (96%) of crude ethyl 2-fluorocinnamate. This material was used without further purification.

후처리

  1. temperatureto reflux for 48 h
  2. concentrationThe mixture was concentrated in vacuo
  3. washwashed successively with a 5% aqueous sodium bicarbonate solution, water and brine
  4. dry with materialdried (Na2SO4)
  5. filtrationFiltration and concentration

출처 및 근거

ORD 기록
ord-779241cd286b412d9ca627535625ecf0
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05872118

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