3-chloro-5-[3-(trifluoromethyl)-1H-pyrazol-1-yl]-2-pyridineacetonitrile → 3-chloro-5-[3-(trifluoromethyl)-1H-pyrazol-1-yl]-2-pyridineethanamine

HRID 2408233ノート

反応式

HRID 2408233 の反応式
[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

  1. filtrationThe mixture was filtered through a pad of Celite® diatomaceous filter aid
  2. washthe filter pad was washed with dichloromethane
  3. 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

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