Triethylamine → HCID 14100224, compound

Participants

Reaction Steps

To a stirred solution of 2.7 grams (0.021 mole) of 3,5-difluoroaniline in 100 ml of dioxane was added via syringe 1.5 ml (0.013 mole ) of trichloromethyl chloroformate. The reaction mixture was heated under reflux for 18 hours, cooled to ambient temperature, and 2.0 grams (0.021 mole) of 4-aminopyridazine and 7.01 ml (0.05 mole) of triethylamine were added. The reaction mixture was heated at 50° C. for one day, cooled to ambient temperature and filtered. The filter cake was washed with dioxane and dried. The solid was slurried in hot water for one hour. The mixture was filtered and the filter cake dried to give 4.1 grams of N-(4-pyridazinyl)-N'-(3,5-difluorophenyl)urea; m.p. 272°-273° C. The nmr spectrum was consistent with the proposed structure.

Provenance & Evidence