Hydrazine → 4-Cyano-4-phenylpiperidine propylamine

HRID 324330

반응식

HRID 324330 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 98377104-Cyano-4-phenylpiperidine propylamine수율 96%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-48eb091d8e834b66866f57d0bee1dd1d
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06218390B1

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