Ammonia → HCID 22251304, compound

Participants

Reaction Steps

At room temperature, NH3 (20 mL, 135 mmol, 7N in methanol) was added subsurface via syringe to a stirred slurry of semicarbazide hydrochloride (10.0 g, 90 mmol) in methanol (75 mL). After one hour, the solution was filtered to remove ammonium chloride. The filtrate was diluted with ethyl acetate (150 mL) and the resulting solution was concentrated to ˜300 mL by a reduced pressure distillation. The solution was filtered and treated with toluene sulfonic acid (17.1 g, 90 mmol). Upon acid addition, a white precipitate formed which was collected by filtration. The solid was rinsed with ethyl acetate (50 mL) and dried under reduced pressure.

Provenance & Evidence