反应详情

温度

70 °C

To a suspension of N-(4-methyl-5-(4-methylpyridin-2-yl)thiazol-2-yl)thiourea (529 mg) in N,N-dimethylformamide (10 ml) were added a solution of hydrogen chloride in 1,4-dioxane (4N, 1 ml) and iodoethane (0.8 ml), and the mixture was stirred at 70° C. for 4 hours. Ethyl acetate (100 ml) was added to the mixture, and the mixture was cooled. The precipitate was collected by filtration and purified by column chromatography (silica gel, triethylamine:methanol:dichloromethane=1:2:100). The combined fractions were evaporated under reduced pressure, and the residue was dissolved in ethyl acetate (5 ml). To the solution was added a solution of hydrogen chloride in 1,4-dioxane (4N, 1.25 ml). The precipitate was collected by filtration and dried under reduced pressure to give N-(4-methyl-5-(4-methylpyridin-2-yl)thiazol-2-yl)-S-ethylisothiourea dihydrochloride (0.69 g).

1. temperaturethe mixture was cooled
2. filtrationThe precipitate was collected by filtration
3. custompurified by column chromatography (silica gel, triethylamine:methanol:dichloromethane=1:2:100)
4. customThe combined fractions were evaporated under reduced pressure
5. dissolutionthe residue was dissolved in ethyl acetate (5 ml)
6. additionTo the solution was added a solution of hydrogen chloride in 1,4-dioxane (4N, 1.25 ml)
7. filtrationThe precipitate was collected by filtration
8. customdried under reduced pressure