HRID703439

反应详情

EQUATION

反应方程式

HRID 703439 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,2-Dihyrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepin-6-thione (4 g), propargylamine (1.2 ml), n-butanol (100 ml) and a catalytic amount of p-toluenesulfonic acid were combined and refluxed overnight. The reaction mixture was concentrated under reduced pressure. The residue was purified by high performance liquid chromatography (2% methanol/dichloromethane) to give 3.1 g (71.4%) of product. Recrystallization from ethanol gave the analytical sample, mp 175° C.

WORKUP

后处理

  1. temperaturerefluxed overnight
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customThe residue was purified by high performance liquid chromatography (2% methanol/dichloromethane)