HRID430654

反应详情

EQUATION

反应方程式

HRID 430654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
112.5 °C

PROCEDURE

实验过程

1.17 g (2.78 mmol) of the compound of step B is dissolved in 40 ml of anhydrous DMF and mixed with 0.73 g (8.4 mmol) of butyric acid hydrazide as well as 3 drops of concentrated HCl. The mixture is stirred for 5 hours at 110-115° C. Then, the mixture is poured onto ice (160 g) and stirred for 1 more hour. The precipitated crystals are suctioned off and washed with water. 1.05 g (83%) of 9-bromo-6-(4-nitrophenyl)-8-methoxy-3-propyl-11H-[1,2,4]triazolo(4,3-c][2,3]benzodiazepine with a melting point of 238-240° C. is obtained.

WORKUP

后处理

  1. additionThen, the mixture is poured onto ice (160 g)
  2. stirringstirred for 1 more hour
  3. washwashed with water