HRID962461

反应详情

EQUATION

反应方程式

HRID 962461 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

Benzoyl chloride (25.8 ml) in dichloromethane (20 ml) was added dropwise over 30 minutes to a mixture of 4-(2-hydroxyethyl)piperidine (26 g) in dichloromethane (250 ml) and triethylamine (16.3 ml) at 0° C. The mixture was allowed to warm to ambient temperature and stirred at this temperature for 1 hour. The mixture was washed with sodium bicarbonate solution and then dried and evaporated to give a colourless oil. The oil was dissolved in 1,4-dioxane (250 ml) and then a solution of sodium hydroxide (5.0 g) in water (20 ml) was added and the mixture stirred at ambient temperature for 16 hours and then at 60° C. for 6 hours. The mixture was evaporated to near dryness, basified with 2M sodium hydroxide solution and the product extracted into dichloromethane to give 1-benzoyl-4-(2-hydroxyethyl)piperidine as an oil.

WORKUP

后处理

  1. washThe mixture was washed with sodium bicarbonate solution
  2. customdried
  3. customevaporated
  4. customto give a colourless oil
  5. stirringthe mixture stirred at ambient temperature for 16 hours
  6. waitat 60° C. for 6 hours
  7. customThe mixture was evaporated
  8. extractionthe product extracted into dichloromethane