Phosgene → 5-Methoxy-1,3,4-thiadiazol-2-yl isocyanate

A saturated solution of phosgene in ethyl acetate (100 ml) is charged into a glass reaction vessel equipped with a mechanical stirrer. A slurry of 5-methoxy-2-amino-1,3,4-thiadiazole (40 grams) in ethyl acetate (300 ml) is added to the reaction vessel, and the resulting mixture is stirred for a period of about 16 hours, resulting in the formation of a precipitate. The reaction mixture is then purged with nitrogen as to remove unreacted phosgene. The purged mixture is then filtered to recover the precipitate. The precipitate is then recrystallized to yield the desired product 5-methoxy-1,3,4-thiadiazol-2-yl isocyanate dimer.

1. customequipped with a mechanical stirrer
2. customresulting in the formation of a precipitate
3. customThe reaction mixture is then purged with nitrogen as
4. customto remove unreacted phosgene
5. filtrationThe purged mixture is then filtered
6. customto recover the precipitate
7. customThe precipitate is then recrystallized

ORD record

ord-ed497309a44b42b2a10ea79a8b8fc982

Source dataset

uspto-grants-1977_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04052191