Sodium Bicarbonate → HCID 20367576, compound

Participants

Reaction Steps

A stirred mixture of 8.5 g of 1-methyl-3-(4-cyano-3-(diethylamino)-5-isothiazolyl)urea in 17 ml of concentrated sulfuric acid was heated at 100° during 11/4 hours. The reaction mixture was poured into 250 ml of stirred ice-water. The mixture became unstirrable and was then carefully poured into 1 liter of saturated sodium bicarbonate solution. The mixture was stirred during one and a quarter hours, filtered cold, and washed with cold water. The collected solid was recrystallized twice from ethanol to give 5.3 g of 1-methyl-3-(4-carbamoyl-3-(diethylamino)-5-isothiazolyl)urea; m.p. 195°-197°. The nmr spectrum was consistent with the assigned structure.

Provenance & Evidence