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

HRID 362827

反応式

HRID 362827 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-779241cd286b412d9ca627535625ecf0
出典データセット
uspto-grants-1999_02
特許番号
US05872118

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