HRID372086

反应详情

EQUATION

反应方程式

HRID 372086 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-(β-phenylethyl)morpholine-5-one (430 mg.) in dry tetrahydrofuran (4 ml.) is added to a stirred suspension of lithium aluminium hydride (200 mg.) in dry ether (20 ml.) at such a rate that the mixture refluxes gently. After complete addition, the mixture is stirred and refluxed for 2 hours, then it is cooled and there are successively added water (0.2 ml.), sodium hydroxide solution (2N, 0.2 ml.) and water (0.6 ml.) and stirring is continued for 15 minutes. The mixture is filtered and the filtrate is evaporated under reduced pressure to give 2-(β-phenylethyl)morpholine as an oil which may be converted to its hydrogen oxalate salt, m.p. 151°-152° C. or its hydrogen maleate salt, m.p. 120°-122° C. on recrystallisation from methanol/ethyl acetate.

WORKUP

后处理

  1. additionAfter complete addition
  2. temperaturerefluxed for 2 hours
  3. temperatureit is cooled
  4. stirringstirring
  5. filtrationThe mixture is filtered
  6. customthe filtrate is evaporated under reduced pressure