Hydrazine → 4-Cyano-4-phenylpiperidine propylamine

HRID 278922

反応式

HRID 278922 の反応式
[C:1]([C:3]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH2:8][CH2:7][N:6]([CH2:9][CH2:10][CH2:11]C2C=CC=C3C(NC(=O)C=23)=O)[CH2:5][CH2:4]1)#[N:2].[NH2:29]N>CO>[C:1]([C:3]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH2:8][CH2:7][N:6]([CH2:9][CH2:10][CH2:11][NH2:29])[CH2:5][CH2:4]1)#[N:2]

参加物

4

反応物 2

HCID 9321HydrazineHCID 227252233-(4-Cyano-4-phenylpiperidin-1-yl)propylphthalimide

生成物 1

HCID 98377104-Cyano-4-phenylpiperidine propylamine収率 96%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 3-(4-cyano-4-phenylpiperidin-1-yl)propylphthalimide (112 g, 0.3 mol) in methanol (1.5 L), hydrazine (30 mL) was added and the mixture was stirred and refluxed for 20 hours. It was cooled, the white solid formed was filtered and washed with more methanol (200 mL). Solvent was evaporated from the filtrate and residue was dried under vacuum for 4 hours. Chloroform (500 mL) was added to this, stirred for 1 hour and filtered. The white solid was washed with more chloroform (200 mL), the solvent was evaporated from the combined filtrates to leave the product as an oil (70 g, 96%).

後処理

  1. temperaturerefluxed for 20 hours
  2. temperatureIt was cooled
  3. customthe white solid formed
  4. filtrationwas filtered
  5. washwashed with more methanol (200 mL)
  6. customSolvent was evaporated from the filtrate and residue
  7. customwas dried under vacuum for 4 hours
  8. additionChloroform (500 mL) was added to this,
  9. stirringstirred for 1 hour
  10. filtrationfiltered
  11. washThe white solid was washed with more chloroform (200 mL)
  12. customthe solvent was evaporated from the combined filtrates

出典と根拠

ORDレコード
ord-b8e4be3515b84f4e9cee3d151f9cb46b
出典データセット
uspto-grants-2002_03
特許番号
US06362182B1

関連ノート

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