HRID324328
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturerefluxed for 20 hours
- temperatureIt was cooled
- customthe white solid formed
- filtrationwas filtered
- washwashed with more methanol (200 mL)
- customSolvent was evaporated from the filtrate and residue
- customwas dried under vacuum for 4 hours
- additionChloroform (500 mL) was added to this,
- stirringstirred for 1 hour
- filtrationfiltered
- washThe white solid was washed with more chloroform (200 mL)
- customthe solvent was evaporated from the combined filtrates