Phosgene → 1,3,4-Thiadiazole, 2-isocyanato-5-(trifluoromethyl)-, dimer

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 (45 grams) 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 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-2-yl isocyanate dimer.

1. customequipped with a mechanical stirrer
2. customresulting in the formation of 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

ORDレコード

ord-1236806236344481b55dfe79995273e2

出典データセット

uspto-grants-1977_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04036848