Hydrogen Sulfide → HCID 20138267, compound

Temperature

0 °C

Hydrogen sulfide was bubbled to a solution of 1.4 gm (11.5 mmole) of N-methyl-2-cyanomethylimidazole and 10 ml dry pyridine stirred in a medium pressure glass Carius tube at 0° C. Then 1.5 equivalents of triethylamine was added (2.50 ml) and the pressure tube was sealed and heated on a steam bath for 4 hours. It was cooled and cracked open to vent any excess hydrogen sulfide. The product crystallized out of the solution when it was cooled to 0° C. The crystals were filtered and washed with 2×5 ml of hexane to afford 1.29 gm of N-methyl-2-thioacetamidioimidazole, m.p. 155°-160° C. (decomposition).

1. customthe pressure tube was sealed
2. temperatureheated on a steam bath for 4 hours
3. temperatureIt was cooled
4. customThe product crystallized out of the solution when it
5. temperaturewas cooled to 0° C
6. filtrationThe crystals were filtered
7. washwashed with 2×5 ml of hexane
8. customto afford 1.29 gm of N-methyl-2-thioacetamidioimidazole, m.p. 155°-160° C. (decomposition)

ORD record

ord-c4a807da85854d3895181b7918e89ce5

Source dataset

uspto-grants-1988_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04746669