HRID47331
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
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
- temperatureunder ice-cooling
- temperatureheated
- temperatureunder reflux for 1 hr and 20 min
- customAfter evaporating
- addition50 ml methanol was added
- temperatureit was heated
- temperatureunder reflux for 1 hr
- customThe reaction solution was evaporated
- washthe crystalline residue was washed with ethyl acetate
- filtrationcollected by filtration