反应详情

3-Aminomethyl-4-(3-(2-chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazole di-p-toluenesulfonate (7.40 g) was dissolved in dichloroethane (100 ml). 2-Chlorophenyl isocyanate (1.2 ml) and triethylamine (4.2 ml) were added under ice-cooling, and the mixture was stirred for 4 hours. Then, the reaction mixture was washed with water and dried over magnesium sulfate. The solvent was evaporated, and the residue was purified by silica gel column chromatography (developing solvent:chloroform -methanol) to give 4.50 g of N-(4-(3-(2-chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazol-3-ylmethyl)-N'-(2-chlorophenyl)urea as an oil.

1. temperaturecooling
2. washThen, the reaction mixture was washed with water
3. dry with materialdried over magnesium sulfate
4. customThe solvent was evaporated
5. customthe residue was purified by silica gel column chromatography (developing solvent:chloroform -methanol)