反应详情

温度

37.5 °C

2,5-Dihydroxy-1,4-dithiane (76 g) and cyanoacetamide (84 g) were added to a mixture of methanol (180 mL), water (10 mL) and triethylamine (10 g). The resulting mixture was heated at 35-40° C. for about 30 minutes while stirring, and then heated to 50-60° C. for an additional 30 minutes with stirring. The reaction mixture was then cooled to room temperature and poured into a mixture of ice (100 g)/water (360 mL). A fine precipitate formed upon addition, which was filtered and dried overnight to give 100.6 g of the title compound as a pale gray powder ((M+H)+=143, M.P.=159.0-159.6° C.).

1. temperatureheated to 50-60° C. for an additional 30 minutes
2. stirringwith stirring
3. temperatureThe reaction mixture was then cooled to room temperature
4. customA fine precipitate formed upon addition, which
5. filtrationwas filtered
6. customdried overnight