3-Chloro-2-(trifluoromethyl)phenylacetonitrile → 2-(3-Chloro-2-(trifluoromethyl)phenyl)ethanamine

HRID 1749490ノート

反応式

HRID 1749490 の反応式
[Cl:1][C:2]1[C:3]([C:11]([F:14])([F:13])[F:12])=[C:4]([CH2:8][C:9]#[N:10])[CH:5]=[CH:6][CH:7]=1>CO.[Ni]>[Cl:1][C:2]1[C:3]([C:11]([F:12])([F:13])[F:14])=[C:4]([CH2:8][CH2:9][NH2:10])[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 1

HCID 1181621683-Chloro-2-(trifluoromethyl)phenylacetonitrile

生成物 1

HCID 1181622402-(3-Chloro-2-(trifluoromethyl)phenyl)ethanamine収率 14.8%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

To a solution of 2-(3-chloro-2-(trifluoromethyl)phenyl)acetonitrile (0.10 g, 3.03 mmol) in MeOH (5 mL) was added Raney-nickel (100 mg). The mixture was degassed under vacuum for 10 min, and then hydrogenated under a fully-inflated balloon at room temperature overnight. The mixture was filtered through a pad of celite and the cake was washed with MeOH (10 mL). The filtrate was concentrated under vacuum to give the crude product (100 mg). MS (ESI) m/z 224.1 [M+H]+.

後処理

  1. customThe mixture was degassed under vacuum for 10 min
  2. filtrationThe mixture was filtered through a pad of celite
  3. washthe cake was washed with MeOH (10 mL)
  4. concentrationThe filtrate was concentrated under vacuum

出典と根拠

ORDレコード
ord-c20b56427e8742739678e9fe367a72fb
出典データセット
uspto-grants-2015_10
特許番号
US09156798B2

反応ノート

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