HRID1087043

反应详情

EQUATION

反应方程式

HRID 1087043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.19 g (20 mmoles) 5-chloroacetyl-3H-indol-2-one 4 g dry sodium carbonate, 4.27 g (20 mmoles) 4-phenoxypiperidine hydrochloride and 100 ml ethanol is heated under reflux fo 1 h 15 min under an argon atmosphere. The mixture is left to cool, 10 ml water, then 8 g potassium borohydride are added and stirring is continued for 2 h 30 min at ambient temperature. A further 200 ml water are added, the mixture is stirred for 30 min and filtered, and the solid is washed with water and dried. 4.67 g of oohre orystals are obtained, which are purified by chromatography on a silica column, eluting with a 95/5 mixture of dichloromethane/ methanol.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux
  3. waitThe mixture is left
  4. temperatureto cool
  5. waitis continued for 2 h 30 min at ambient temperature
  6. stirringthe mixture is stirred for 30 min
  7. filtrationfiltered
  8. washthe solid is washed with water
  9. customdried
  10. custom4.67 g of oohre orystals are obtained
  11. customwhich are purified by chromatography on a silica column
  12. washeluting with a 95/5 mixture of dichloromethane/ methanol