HRID66577

反应详情

EQUATION

反应方程式

HRID 66577 的结构方程式

PROCEDURE

实验过程

To a solution of 2-(2-methylguanidino)-4-(3-aminocyclohexyl)thiazole (0.2 g.) in acetonitrile (20 ml.) was added 1,1-di(methylthio)-2-nitroethylene (0.125 g.) and the mixture heated under reflux for 7 hours. The reaction mixture was evaporated to dryness and the residue of 1-[3-[2-(2-methylguanidino)thiazol-4-yl]cyclohexylamino]-1-methylthio-2-nitroethylene, dissolved in ethanol (20 ml.), was treated with 20 ml. of a solution of methylamine in ethanol (33% w/v). The reaction mixture was allowed to stand overnight. Evaporation of the solvent and recrystallisation of the residue from methanol gave 1-[3-[2-(2-methylguanidino)thiazol-4-yl]cyclohexylamino]-1-methylamino-2-nitroethylene, m.p. 164°-174° (decomp.).

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 7 hours
  3. customThe reaction mixture was evaporated to dryness
  4. dissolutionthe residue of 1-[3-[2-(2-methylguanidino)thiazol-4-yl]cyclohexylamino]-1-methylthio-2-nitroethylene, dissolved in ethanol (20 ml.)
  5. additionwas treated with 20 ml
  6. customEvaporation of the solvent and recrystallisation of the residue from methanol