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Ethanol → Ethyl 3-(2,4-difluorophenyl)prop-2-enoate

HRID 612946
ノート
印刷プレビュー

反応式

HRID 612946 の反応式
[F:1][C:2]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:3]=1[CH:4]=[CH:5][C:6]([OH:8])=[O:7].S(=O)(=O)(O)O.[CH2:19](O)[CH3:20]>>[CH2:19]([O:7][C:6](=[O:8])[CH:5]=[CH:4][C:3]1[CH:9]=[CH:10][C:11]([F:13])=[CH:12][C:2]=1[F:1])[CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 6035023-(2,4-Difluorophenyl)acrylic Acid

生成物 1

HCID 53395691Ethyl 3-(2,4-difluorophenyl)prop-2-enoate収率 97%

実験手順

2,4-Difluorocinnamic acid (10.1 g) was dissolved in ethanol (100 ml), and conc. sulfuric acid (1 ml) was added thereto, and the resulting mixture was refluxed for 3 hours. The solvent was evaporated under reduced pressure and the residue was poured into ice-cold water and extracted with ethyl acetate. The extract was washed successively with 5% aqueous sodium hydrogencarbonate and a saturated aqueous NaCl solution, and the organic layer was dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure to obtain the title compound (11.2 g, 97%) as a colorless oil.

後処理

  1. temperaturethe resulting mixture was refluxed for 3 hours
  2. customThe solvent was evaporated under reduced pressure
  3. additionthe residue was poured into ice-cold water
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed successively with 5% aqueous sodium hydrogencarbonate
  6. dry with materiala saturated aqueous NaCl solution, and the organic layer was dried over anhydrous magnesium sulfate
  7. filtrationAfter filtration
  8. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-edcfeb9509c1427793abc0199299ed2d
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06005116

反応ノート

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