Ammonia → 4-Amino-1-(1-phenyl-ethyl)-piperidine-4-carbonitrile

HRID 2365584ノート

反応式

HRID 2365584 の反応式
[C:1]1([CH:7]([N:9]2[CH2:14][CH2:13][C:12](=O)[CH2:11][CH2:10]2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-].[NH4+:17].[NH3:18].[C-:19]#N.[Na+]>O>[NH2:17][C:12]1([C:19]#[N:18])[CH2:13][CH2:14][N:9]([CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH3:8])[CH2:10][CH2:11]1

参加物

6

反応物 4

HCID 222AmmoniaHCID 8929Sodium CyanideHCID 25517Ammonium ChlorideHCID 119596271-(1-Phenylethyl)piperidin-4-one

生成物 1

HCID 671207084-Amino-1-(1-phenyl-ethyl)-piperidine-4-carbonitrile

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a mixture of 1-(1-phenyl-ethyl)-piperidin-4-one (10.9 g, 53.6 mmol), ammonium chloride (4.3 g, 80.4 mmol) and 30% aqueous ammonia solution (30 ml) in water (30 ml) at room temperature is added sodium cyanide (4.0 g, 81.6 mmol) portion wise. The reaction mixture is stirred at room temperature for 18 hours, then diluted with water and extracted with DCM. The organic phase is washed with brine, dried over Na2SO4, filtered and concentrated in vacuo to obtain 4-Amino-1-(1-phenyl-ethyl)-piperidine-4-carbonitrile as a brown oil; [M+H]+ 230.

後処理

  1. extractionextracted with DCM
  2. washThe organic phase is washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-88754d1a6a7141ffa9317a57c3229610
出典データセット
uspto-grants-2014_04
特許番号
US08697687B2

反応ノート

読み込み中…