HRID1646384

反应详情

EQUATION

反应方程式

HRID 1646384 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customthe methanol is stripped off on a rotary evaporator
  2. extractionthe solution is extracted with dichloromethane
  3. washThe combined organic phases are washed with water of pH 5
  4. additioncontaining acetic acid
  5. customdried
  6. concentrationconcentrated
  7. customwhich are employed in the following step without further purification