HRID1731576

反应详情

EQUATION

反应方程式

HRID 1731576 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-[2-(4-methoxyphenyl)ethyl]-2-hydroxy-1-oxo-2-(3-chlorophenyl)ethanamine (2.8 g) in dry tetrahydrofuran (20 ml) was added slowly to a refluxing suspension of lithium aluminium hydride (1.36 g) in tetrahydrofuran (30 ml) at reflux and then heated under reflux for 24 hours. After careful addition of water (1.4 ml), aqueous sodium hydroxide (10%; 1.4 ml) and water (2.8 ml), filtration and evaporation of the filtrate gave the crude product. Recrystallisation from ethyl acetate-hexane gave N-[2-(4-methoxyphenyl)-ethyl]-2-hydroxy-2-(3-chlorophenyl)ethanamine, mp 101°-3° C.

WORKUP

后处理

  1. temperatureat reflux
  2. temperatureheated
  3. temperatureunder reflux for 24 hours
  4. customgave the crude product
  5. customRecrystallisation from ethyl acetate-hexane