反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturethe mixture heated
- temperatureunder reflux for 7 hours
- customThe reaction mixture was evaporated to dryness
- dissolutionthe residue of 1-[3-[2-(2-methylguanidino)thiazol-4-yl]cyclohexylamino]-1-methylthio-2-nitroethylene, dissolved in ethanol (20 ml.)
- additionwas treated with 20 ml
- customEvaporation of the solvent and recrystallisation of the residue from methanol