HRID262992

反应详情

EQUATION

反应方程式

HRID 262992 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1 g of 7-chloro-5-(o-chlorophenyl)-1,3-dihydro-2H-thieno[2,3-e]-1,4-diazepine-2-thione is refluxed for 1.5 hours in 50 ml of absolute methanol with 2 g of lactic acid hydrazide. The precipitated 7-chloro-5-(o-chlorophenyl)-2-(2-lactoylhydrazino)-3H-thieno[2,3-e]-1,4-diazepine is dried and refluxed for 4 hours in 120 ml of absolute xylene. The solution is evaporated and the product recrystallized from ethyl acetate containing active carbon to yield 2-chloro-4-(o-chlorophenyl)-9-(α-hydroxyethyl)-6H-thieno[3,2-f]-s- triazolo[4,3-a][1,4]diazepine of melting point 118°-120° C.

WORKUP

后处理

  1. dry with materialThe precipitated 7-chloro-5-(o-chlorophenyl)-2-(2-lactoylhydrazino)-3H-thieno[2,3-e]-1,4-diazepine is dried
  2. temperaturerefluxed for 4 hours in 120 ml of absolute xylene
  3. customThe solution is evaporated
  4. customthe product recrystallized from ethyl acetate containing active carbon