反应详情

To a stirred slurry of 126 g of 2-methylamino-5-mercapto-1,3,4-thiadiazole in 525 ml of dioxane containing a few drops of triethylamine is added 49 g of methyl isocyanate. After stirring two hours at room temperature, the solid is collected by filtration and washed with hexane giving 165 g, melting at 162°-3°. This product is heated on the steam bath 11/2 -2 hours with 250 ml of triethylamine, during which time the initial solid is converted to a heavy amber oil. The supernatent liquid is decanted and the oil is dissolved in water and neutralized with dilute hydrochloric acid to pH 2-3. The precipitated solid is collected and washed with water and air dried, giving 132 g of N,N'-dimethyl-N'-(5-mercapto-1,3,4-thiadiazol-2-yl)urea, m.p. 230° (dec.).

1. filtrationthe solid is collected by filtration
2. washwashed with hexane giving 165 g, melting at 162°-3°
3. temperatureThis product is heated on the steam bath 11/2 -2 hours with 250 ml of triethylamine
4. customThe supernatent liquid is decanted
5. dissolutionthe oil is dissolved in water and neutralized with dilute hydrochloric acid to pH 2-3
6. customThe precipitated solid is collected
7. washwashed with water and air
8. customdried