1,1,1-Trifluoro-3-nitro-2-pentanol → 3-Amino-1,1,1-trifluoropentan-2-ol
反応式
[F:1][C:2]([F:12])([F:11])[CH:3]([OH:10])[CH:4]([N+:7]([O-])=O)[CH2:5][CH3:6]>CO.[Ni]>[NH2:7][CH:4]([CH2:5][CH3:6])[CH:3]([OH:10])[C:2]([F:12])([F:11])[F:1]参加物
4
実験手順
1,1,1-trifluoro-3-nitropentan-2-ol (3 g, 16 mmol) was dissolved in methanol (40 ml). Raney Nickel catalyst was added and the reaction vigorously stirred under an atmosphere of hydrogen for 24 h. The catalyst was filtered and the filtrate was concentrated in vacuo to give the amine relatively pure (2.35 g, 94%). δH (CDCl3, 500 MHz) 1.05 (3 H, t, J 5, CHCH2CH3), 1.55-1.45 (1 H, m, CHCHHCH3), 1.8-1.7 (1 H, m, CHCHHCH3), 2.95-2.9 (1 H, m, CHEt), 3.95-3.85 (1 H, m, CHOHCF3); δC (CDCl3, 500 MHz) 124.5 (C), 71.5 (CH), 54.03 (CH), 25.5 (CH2), 11.05 (CH3)
後処理
- customthe reaction
- filtrationThe catalyst was filtered
- concentrationthe filtrate was concentrated in vacuo
出典と根拠
- ORDレコード
- ord-c454522ae63d4862a6e517d085ba927e
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08592581B2
反応ノート
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