HRID27382

反应详情

EQUATION

反应方程式

HRID 27382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-nitro-2-methylthio-2-{2-[(4-methyl-1H-imidazol-5-yl)methylthio]ethylamino}ethylene (3.13 g, 10.9 mmole) and 3-amino-1-butyne (4.5 g, 65.1 mmole) in acetonitrile (45 ml) was stirred at reflux temperature under a positive pressure of nitrogen for 17 hours. The reaction mixture was evaporated under reduced pressure then the residue placed on silica gel and chromatographed by gradient elution using methylene chloride-methanol. Recrystallization yielded the title compound.

WORKUP

后处理

  1. temperatureat reflux temperature under a positive pressure of nitrogen for 17 hours
  2. customThe reaction mixture was evaporated under reduced pressure
  3. customchromatographed by gradient elution
  4. customRecrystallization