Water → 1H-Inden-1-one, 4-bromo-2,3-dihydro-5-(trifluoromethyl)-

HRID 471459ノート

反応式

HRID 471459 の反応式
[Br:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:12][CH2:13][C:14]([OH:16])=O.O>FC(F)(F)S(O)(=O)=O>[Br:1][C:2]1[C:7]([C:8]([F:9])([F:10])[F:11])=[CH:6][CH:5]=[C:4]2[C:3]=1[CH2:12][CH2:13][C:14]2=[O:16]

参加物

4

反応物 2

HCID 962WaterHCID 53808869Benzenepropanoic acid, 2-bromo-3-(trifluoromethyl)-

生成物 1

HCID 867007731H-Inden-1-one, 4-bromo-2,3-dihydro-5-(trifluoromethyl)-

試薬・触媒・溶媒 1

HCID 62406Trifluoromethanesulfonic acid溶媒

反応条件

温度
85 °C

実験手順

3-(2-Bromo-3-trifluoromethyl-phenyl)-propionic acid (3.0 g, 10.1 mmol) is suspended in trifluoromethanesulfonic acid (30 mL)) under argon and heated at 85° C. for 4 hours. The mixture is added dropwise to iced water and then extracted with ethyl acetate. The organic extract is washed with saturated sodium bicarbonate solution, dried and concentrated under vacuum. The residue is purified by flash chromatography (Eluent 0-5% EtOAc in cyclohexane) to give the title compound.

後処理

  1. extractionextracted with ethyl acetate
  2. extractionThe organic extract
  3. washis washed with saturated sodium bicarbonate solution
  4. customdried
  5. concentrationconcentrated under vacuum
  6. customThe residue is purified by flash chromatography (Eluent 0-5% EtOAc in cyclohexane)

出典と根拠

ORDレコード
ord-962ec0282eea4bd1935c15bb6dfbed29
出典データセット
uspto-grants-2014_01
特許番号
US08633182B2

反応ノート

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