反应详情

2,6-Diisopropylphenylisocyanate (1.9 g, 9.4 mmol) was added to a refluxing solution of 5-amino-3-phenyl-1,2,4-thiadiazole (1.5 g, 8.5 mmol) in acetonitrile (60 mL). The mixture was refluxed for 18 hours, allowed to cool, filtered, and the filtrate concentrated, taken up in ethyl acetate (150 mL), and washed with water (3×50 mL). The organics were dried over Na2SO4, filtered, concentrated, and the resulting solid washed with hexane and recrystallized from acetonitrile to give a white solid (1.50 g, 46%), m.p. 180°-183° C.

1. temperatureThe mixture was refluxed for 18 hours
2. temperatureto cool
3. filtrationfiltered
4. concentrationthe filtrate concentrated
5. washwashed with water (3×50 mL)
6. dry with materialThe organics were dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated
9. washthe resulting solid washed with hexane
10. customrecrystallized from acetonitrile