HRID1275363

反应详情

EQUATION

反应方程式

HRID 1275363 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 1 g N-(2-chloro-5-thiazolylmethyl)-S-methyl-N'-nitroisothiourea, 560 mg potassium carbonate, 400 mg cuprous chloride and 12 ml acetonitrile was added 610 mg of 2-chloro-5-(aminomethyl)thiazole and the mixture was stirred for 1 hour under reflux. Thereafter, the reaction mixture was concentrated, then water was added to the resultant solids, followed by stirring thoroughly. Thereafter, the solids were collected by filtration and purified by column chromatography [eluent: dichloromethane-methanol (10:1)] to afford 191 mg of N,N'-bis(2-chloro-5-thiazolylmethyl)-N"-nitroguanidine (compound No.39) as a white powder, mp 217-218° C.

WORKUP

后处理

  1. temperatureunder reflux
  2. concentrationThereafter, the reaction mixture was concentrated
  3. additionwater was added to the resultant solids
  4. stirringby stirring thoroughly
  5. filtrationThereafter, the solids were collected by filtration
  6. custompurified by column chromatography [eluent: dichloromethane-methanol (10:1)]