HRID2291559

反应详情

EQUATION

反应方程式

HRID 2291559 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(2-Chloro-4-nitrophenyl)-4-(4-nitrophenethyl)piperazine (1.0 g), stannous chloride dihydrate (5.7 g) and ethanol (50 ml) were stirred under reflux for 1.25 hours, the mixture was evaporated to low bulk, and added to aqueous 5% sodium hydroxide (100 ml). The mixture was then extracted three times with dichloromethane and the combined organic extracts were dried (sodium sulphate) and evaporated to yield a yellow oil which solidified: yield of the title compound 0.6 g, m.p. 109°-112°. It was used in the next stage without further purification.

WORKUP

后处理

  1. temperatureunder reflux for 1.25 hours
  2. customthe mixture was evaporated to low bulk
  3. additionadded to aqueous 5% sodium hydroxide (100 ml)
  4. extractionThe mixture was then extracted three times with dichloromethane
  5. dry with materialthe combined organic extracts were dried (sodium sulphate)
  6. customevaporated
  7. customto yield a yellow oil which