Ammonia → HCID 86603523, compound

Participants

Reaction Steps

At room temperature, NH3 (96 mL, 670 mmol, 7N in methanol) was added subsurface via syringe to a stirred slurry of semicarbazide hydrochloride (50 g, 450 mmol) in methanol (375 mL). After one hour, the solution was filtered to remove ammonium chloride. The filtrate was diluted with ethyl acetate (750 mL) and the resulting solution was concentrated to ˜400 mL by a reduced pressure distillation. The solution was filtered and treated with methane sulfonic acid (47.4 g, 490 mmol). Upon acid addition, a white precipitate formed which was collected by filtration. The solid was rinsed with ethyl acetate (200 mL) and dried under reduced pressure.

Provenance & Evidence