HRID567725

反应详情

EQUATION

反应方程式

HRID 567725 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.6 g (11 mmol) of 1-(3,4-dichlorobenzyl)-5-methylthio-1H-indazol-3-ol are dissolved in 100 ml of DMSO and treated in portions with 0.34 g (13.2 mmol) of sodium hydride (95 percent). After stirring for 2 hours, a solution of 2.1 g (11 mmol) of 2-hydroxy-5-nitrobenzyl chloride in 20 ml of DMSO is added dropwise and the mixture is stirred at 60° C. for 3 hours. After cooling, 200 ml of water are added dropwise, the mixture is stirred for 4 hours and the solid is filtered off with suction. The precipitate is extracted by stirring with methanol whilst hot and recrystallized from 2-propanol.

WORKUP

后处理

  1. stirringthe mixture is stirred at 60° C. for 3 hours
  2. temperatureAfter cooling
  3. stirringthe mixture is stirred for 4 hours
  4. filtrationthe solid is filtered off with suction
  5. extractionThe precipitate is extracted
  6. stirringby stirring with methanol whilst hot and
  7. customrecrystallized from 2-propanol