反应详情

A saturated solution of phosgene in ethyl acetate (100 ml) was charged into a glass reaction vessel equipped with a mechanical stirrer. A slurry of 5-trifluoromethyl-2-amino-1,3,4-thiadiazole (45grams) in ethyl acetate (300 ml) was added to the reaction vessel and the resulting mixture was stirred for a period of about 16 hours resulting in the formation of a precipitate. The reaction mixture was then purged with nitrogen gas to remove unreacted phosgene. The purged mixture was filtered to recover 48 grams of a white solid. This solid was recrystallized from dimethyl formamide to yield the desired product 5-trifluoromethyl-1,3,4-thiadiazol-2yl isocyanate dimer.

1. customequipped with a mechanical stirrer
2. customresulting in the formation of a precipitate
3. customThe reaction mixture was then purged with nitrogen gas
4. customto remove unreacted phosgene
5. filtrationThe purged mixture was filtered
6. customto recover 48 grams of a white solid
7. customThis solid was recrystallized from dimethyl formamide