HRID1981970

反应详情

EQUATION

反应方程式

HRID 1981970 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 17.8 g of 7-chloro-1-(β-chloroethyl)-2-chloromethyl-5-(2-furyl)-2,3-dihydro-1H-1,4-benzodiazepine in 250 ml of methylene chloride is heated under reflux with 10.4 g of 3-chloroperbenzoic acid for 2-hours. The reaction solution is then rendered alkaline with aqueous dilute sodium hydroxide solution and is worked upon in the customary manner, and the reaction product is isolated and then purified by chromatography on aluminium oxide of activity level II, using methylene chloride, and crystallised from methanol. 13 g of 7-chloro-1-(β-chloroethyl)- 2-chloromethyl-5-(2-furyl)-2,3-dihydro-1H-1,4-benzodiazepine 4-oxide are obtained. Melting point: 158° to 159° C.

WORKUP

后处理

  1. customthe reaction product is isolated
  2. custompurified by chromatography on aluminium oxide of activity level II
  3. customcrystallised from methanol