Ammonia → 1-(6-Chloropyridin-3-yl)ethan-1-amine
反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8](=O)[CH3:9])=[CH:4][CH:3]=1.[NH3:11].[BH4-].[Na+]>CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-].[Ti+4]>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH:8]([NH2:11])[CH3:9])=[CH:4][CH:3]=1参加物
5
実験手順
Stir a mixture of 1-(6-chloro-pyridin-3-yl)-ethanone (5 g, 32.14 mmol) in titanium tetra(isopropoxide) (18.27 g, 64.27 mmol) and ammonia (160.7 mmol, 2 M in MeOH) under N2 for 6 hours at room temperature. To this mixture add sodium tetrahydroborate (1.82 g, 48.21 mmol) and stir overnight. Quench the reaction mixture with ammonium hydroxide and filter the mixture. From the filtrate remove the solvent and extract the residue with dichloromethane, wash with saturated aqueous sodium chloride and dry over Na2SO4, filter and remove the solvent to obtain a dark yellow oil (4.2 g). MS (ES) m/z 157 [M+1]+.
後処理
- stirringstir overnight
- customQuench the reaction mixture with ammonium hydroxide
- filtrationfilter the mixture
- customFrom the filtrate remove the solvent
- extractionextract the residue with dichloromethane
- washwash with saturated aqueous sodium chloride
- dry with materialdry over Na2SO4
- filtrationfilter
- customremove the solvent
出典と根拠
- ORDレコード
- ord-43ddad6d5af44e18aea4a66ff2af4dde
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063212B2
反応ノート
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