Benzyl 5-cyano-2-(trifluoromethyl)benzoate → 5-(Aminomethyl)-2-(trifluoromethyl)benzoic acid
反応式
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([C:19]([F:22])([F:21])[F:20])=[C:7]([CH:18]=1)[C:8]([O:10]CC1C=CC=CC=1)=[O:9])#[N:2].[H][H]>[Pd].CO>[NH2:2][CH2:1][C:3]1[CH:4]=[CH:5][C:6]([C:19]([F:20])([F:21])[F:22])=[C:7]([CH:18]=1)[C:8]([OH:10])=[O:9]参加物
5
実験手順
Combine benzyl 5-cyano-2-(trifluoromethyl)benzoate (3.9 g, 12.78 mmol, 1.0 equiv), palladium (10 wt % on carbon, 400 mg, 0.38 mmol, 0.03 equiv), and methanol (128 mL), and purge the mixture with hydrogen. Stir overnight under a hydrogen atmosphere. Filter the mixture through a pad of diatomaceous earth, and then rinse the pad with hot methanol (3×150 mL) to bring through precipitated product. Concentrate the filtrate under reduced pressure to give the title compound (1.4 g, 50%). MS (m/z) 220 (M+1).
後処理
- filtrationFilter the mixture through a pad of diatomaceous earth
- washrinse the pad with hot methanol (3×150 mL)
- customto bring through precipitated product
- concentrationConcentrate the filtrate under reduced pressure
出典と根拠
- ORDレコード
- ord-21675f574bca4d0eadccd8c716c51bfa
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08252831B2
反応ノート
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