HRID1415602

反应详情

EQUATION

反应方程式

HRID 1415602 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-[[7-chloro-5-(2-pyridyl)-3H-1,4-benzodiazepin-2-yl]amino]propionaldehyde dimethyl acetal in monoglyme is treated with titanium tetrachloride first at room temperature, then under reflux. The reaction mixure is cooled, neutralized, and extracted with chloroform. The chloroform layer is concentrated in vacuo and the resulting residue crystallized to give 8-chloro-2-methyl-6-(2-pyridyl)-4H-imidazo[1,2-a][1,4]benzodiazepine.

WORKUP

后处理

  1. temperatureunder reflux
  2. temperatureThe reaction mixure is cooled
  3. extractionextracted with chloroform
  4. concentrationThe chloroform layer is concentrated in vacuo
  5. customthe resulting residue crystallized