HRID1646384
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
A solution of 4.9 g of sodium cyanide in 10 ml of water and a solution of 7.2 g of isobutyraldehyde in 30 ml of methanol are added dropwise with ice-cooling to a mixture of 6.4 g of 1-amino-2,6-dimethylpiperidine, 60 ml of water and 8.6 ml of concentrated hydrochloric acid. After stirring at room temperature for 8 days, the methanol is stripped off on a rotary evaporator and the solution is extracted with dichloromethane. The combined organic phases are washed with water of pH 5 containing acetic acid, dried and concentrated. 11.2 g of 2-((2,6-dimethylpiperidino)amino)-3-methylbutyronitrile remain, which are employed in the following step without further purification.
WORKUP
后处理
- customthe methanol is stripped off on a rotary evaporator
- extractionthe solution is extracted with dichloromethane
- washThe combined organic phases are washed with water of pH 5
- additioncontaining acetic acid
- customdried
- concentrationconcentrated
- customwhich are employed in the following step without further purification