HRID845759

反应详情

EQUATION

反应方程式

HRID 845759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A reaction mixture, prepared from 1-[2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-1-methylthio-2-nitroethylene, cyclopropylamine and ethanol, was heated to refluxing temperature for about three hours. The solvent was then removed by evaporation and the resulting residue was chromatographed over silica using a gradient elution technique. The desired compound was eluted with a 5:95 methanol:ethyl acetate solvent mixture. Removal of the solvent yielded N-2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl-N'-cyclopropyl 2-nitro-1,1-ethenediamine which melted at 128.5°-131.5° C. after recrystallization from a methanol/ethyl acetate solvent mixture.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto refluxing temperature for about three hours
  3. customThe solvent was then removed by evaporation
  4. customthe resulting residue was chromatographed over silica using
  5. washa gradient elution technique
  6. washThe desired compound was eluted with a 5:95 methanol
  7. customRemoval of the solvent