HRID2419789

反应详情

EQUATION

反应方程式

HRID 2419789 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 7.80 g. of methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide and 4.37 of 1-phenylcyclopropanemethylamine in 100 ml. of n-butanol and 25 ml. of water is heated at reflux for 24 hours. The solution is cooled, diluted with water to a final volume of 2 liters and is allowed to stand. Filtration gives a tan solid which is dissolved in ethyl acetate and purified by silica gel column chromatography. Crystallization of the product from diethyl ether gives the desired final product as colorless crystals, m.p. 136.5°-138.5° C.

WORKUP

后处理

  1. temperatureat reflux for 24 hours
  2. temperatureThe solution is cooled
  3. filtrationFiltration
  4. customgives a tan solid which
  5. custompurified by silica gel column chromatography
  6. customCrystallization of the product from diethyl ether