反应详情

温度

70 °C

To a suspension of N-(4-methyl-5-(4-methylpyridin-2-yl)thiazol-2-yl)thiourea (1.23 g) in N,N-dimethylformamide were added a solution of hydrogen chloride in 1,4-dioxane (4N, 2.56 ml) and iodoethane (1.86 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=1:5:100) to give N-(4-methyl-5-(4-methylpyridin-2-yl)thiazol-2-yl)-S-ethylisothiourea (1.14 g).

1. temperaturethe mixture was cooled
2. filtrationThe precipitate was collected by filtration
3. custompurified by column chromatography (silica gel, triethylamine:methanol:dichloromethane=1:5:100)