3-chloro-5-[3-(trifluoromethyl)-1H-pyrazol-1-yl]-2-pyridineacetonitrile → 3-chloro-5-[3-(trifluoromethyl)-1H-pyrazol-1-yl]-2-pyridineethanamine
反応式
[Cl:1][C:2]1[C:3]([CH2:17][C:18]#[N:19])=[N:4][CH:5]=[C:6]([N:8]2[CH:12]=[CH:11][C:10]([C:13]([F:16])([F:15])[F:14])=[N:9]2)[CH:7]=1.[H][H]>CO.[Ni]>[Cl:1][C:2]1[C:3]([CH2:17][CH2:18][NH2:19])=[N:4][CH:5]=[C:6]([N:8]2[CH:12]=[CH:11][C:10]([C:13]([F:14])([F:16])[F:15])=[N:9]2)[CH:7]=1参加物
5
実験手順
A solution of 3-chloro-5-[3-(trifluoromethyl)-1H-pyrazol-1-yl]-2-pyridineacetonitrile (i.e. the product of Step B; 5.0 g, 0.017 mol) in methanol (50 mL) was shaken in a Parr hydrogenation apparatus in the presence of Raney nickel (5.0 g) and a hydrogen pressure of 50 psi (345 kPa) at room temperature for 2 h. The mixture was filtered through a pad of Celite® diatomaceous filter aid, and the filter pad was washed with dichloromethane. The filtrate was concentrated under reduced pressure to afford the title compound (2.0 g), which was used without further purification.
後処理
- filtrationThe mixture was filtered through a pad of Celite® diatomaceous filter aid
- washthe filter pad was washed with dichloromethane
- concentrationThe filtrate was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-8a436766c5654e66b5e3e37e0627c609
- 出典データセット
- uspto-grants-2014_08
- 特許番号
- US08815772B2
反応ノート
読み込み中…