HRID47331

反应详情

EQUATION

反应方程式

HRID 47331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11.0 g of 1-benzyl-4-piperidinecarbonitrile was dissolved in 100 ml 1,2-dichloroethane, 7.1 ml 1-chloroethyl chloroformate was added thereto under ice-cooling. The mixture was stirred at room temperature for 15 min, and then heated under reflux for 1 hr and 20 min. After evaporating, 50 ml methanol was added thereto and it was heated under reflux for 1 hr. The reaction solution was evaporated, and the crystalline residue was washed with ethyl acetate and collected by filtration to give 8.0 g of 4-piperidinecarbonitrile hydrochloride as white crystals.

WORKUP

后处理

  1. temperatureunder ice-cooling
  2. temperatureheated
  3. temperatureunder reflux for 1 hr and 20 min
  4. customAfter evaporating
  5. addition50 ml methanol was added
  6. temperatureit was heated
  7. temperatureunder reflux for 1 hr
  8. customThe reaction solution was evaporated
  9. washthe crystalline residue was washed with ethyl acetate
  10. filtrationcollected by filtration