反応式
[N+:1]([CH:4]1[CH2:9][CH2:8][CH2:7][CH2:6][C:5]1=[O:10])([O-])=O.[ClH:11].[H][H]>[Pt].C(O)C>[ClH:11].[NH2:1][CH:4]1[CH2:9][CH2:8][CH2:7][CH2:6][C:5]1=[O:10]参加物
6
実験手順
Add 2-nitrocyclohexanone (7.0 g, 48.9 mmol), 5% platinum sulfided on carbon (500 mg), ethanol (120 mL) and concentrated hydrochloric acid (6 mL) to a pressure vessel under a nitrogen atmosphere. Pressurize the vessel to 50 psi with hydrogen and stir the mixture for 3 h. Filter the mixture through Celite® and wash with ethanol followed by DCM under a nitrogen atmosphere. Concentrate the filtrate in vacuo. Slurry the residue in acetone (50 mL) and filter. Collect the solid to obtain the desired intermediate (2.2 g, 40%).
後処理
- filtrationFilter the mixture through Celite®
- washwash with ethanol
- concentrationConcentrate the filtrate in vacuo
- filtrationfilter
- customCollect the solid
出典と根拠
- ORDレコード
- ord-13a8e41b12f544768e21eb20640b1a6d
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07994163B2
関連ノート
読み込み中…