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

HRID 2406509ノート

反応式

HRID 2406509 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

実験手順

3-(2-Bromo-3-trifluoromethyl-phenyl)-propionic acid (3.25 g) in trifluoromethane-sulfonic acid (30 ml) is stirred at 75° C. for 2.5 h. After cooling to room temperature, the mixture is poured into water and the resulting mixture is extracted with ethyl acetate. The combined organic extract is washed with aqueous NaHCO3 solution, dried (Na2SO4), and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 90:10→80:20) to afford the title compound. LC (method 5): tR=0.90 min.

後処理

  1. extractionthe resulting mixture is extracted with ethyl acetate
  2. extractionThe combined organic extract
  3. washis washed with aqueous NaHCO3 solution
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated
  6. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 90:10→80:20)

出典と根拠

ORDレコード
ord-03cd12b569d944b895e291befb69779e
出典データセット
uspto-grants-2014_08
特許番号
US08809376B2

反応ノート

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