Phosgene → 5-Methylthio-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-methylthio-2-amino-1,3,4-thiadiazole (45 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 gas to remove unreacted phosgene. The purged mixture is then filtered to cover the precipitate. The precipitate is then recrystallized to yield the desired product 5-methylthio-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 gas
4. customto remove unreacted phosgene
5. filtrationThe purged mixture is then filtered
6. customThe precipitate is then recrystallized

ORD record

ord-462a681401074a9a8e00152bd23d50a7

Source dataset

uspto-grants-1977_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04006009