HRID1681831

反应详情

EQUATION

反应方程式

HRID 1681831 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 2.0 g of 4-oxo-4,5,6,7-tetrahydrothieno[2,3-b]thiepin-5-acetic acid and 0.6 g of hydrazine hydrate in 20 ml of ethanol is refluxed under heating for 5 hours. After cooling, the precipitated crystals are collected by filtration and recrystallized from a mixed solvent of chloroform and ethanol to give 1.4 g of 4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one as white crystals, melting at 215°-217° C.

WORKUP

后处理

  1. temperatureis refluxed
  2. temperatureunder heating for 5 hours
  3. temperatureAfter cooling
  4. filtrationthe precipitated crystals are collected by filtration
  5. customrecrystallized from a mixed solvent of chloroform and ethanol