HRID1492232

反应详情

EQUATION

反应方程式

HRID 1492232 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-methyl-1-(2-morpholinophenyl)-2-thiopseudourea (12.5 g) and N-(2-hydroxyethyl)-1,2-dimethylethylenediamine (8 g) in dry ethanol (150 ml) was heated under reflux at 90°-95° C. for 6 days to give a dark brown oil which was purified by column chromatography on neutral alumina (250 g) using a 1:9 mixture of dichloromethane and hexane to give 4-{2-[4,5-dimethyl-1-(2-hydroxyethyl)-2-imidazolidinylideneamino]phenyl}morpholine as a colourless solid (m.p. 108°-109° C.) which was recrystallised from hexane.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux at 90°-95° C. for 6 days
  3. customto give a dark brown oil which
  4. customwas purified by column chromatography on neutral alumina (250 g)
  5. additiona 1:9 mixture of dichloromethane and hexane