HRID127265

反应详情

EQUATION

反应方程式

HRID 127265 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 7 g lithium aluminum hydride and 150 ml tetrahydrofuran under argon is added dropwise over 20 minutes a solution of 24.6 g 8-benzyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one in 150 ml tetrahydrofuran. The mixture is heated at reflux for two hours. The stirred mixture is treated with sequential dropwise additions of 7 ml water, 7 ml 15% sodium hydroxide and 21 ml water. The mixture is filtered and the filter cake is washed with three 200 ml portions of dichloromethane. Evaporation of the combined filtrates affords 23 g of 1-benzyl-4-hydroxy-4-methylaminomethylpiperidine, an oil.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureat reflux for two hours
  3. filtrationThe mixture is filtered
  4. washthe filter cake is washed with three 200 ml portions of dichloromethane
  5. customEvaporation of the combined filtrates