HRID278922

反应详情

EQUATION

反应方程式

HRID 278922 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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%).

WORKUP

后处理

  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