Hydrochloric Acid → HCID 178485177, compound

Participants

Reaction Steps

A mixture of 6-(2-chlorophenyl)-3-methyl-4-oxo-4,5,6,7-tetrahydroindazole (78 mg), 1-amino-3-methylguanidine p-toluenesulfonate (86 mg) and concentrated hydrochloric acid (0.1 ml) in ethanol (1 ml) was stirred at room temperature for 60 hours, and crystals precipitated during the reaction were filtered and washed with ethanol. To the crystals were added ethyl acetate (60 ml) and 2 N sodium hydroxide (5 ml) to dissolve the crystals. The separated ethyl acetate layer was washed with water (10 ml, thrice), to which was added 2 N hydrochloric acid (0.3 ml). The mixture was concentrated under reduced pressure, and the residue was washed with a mixture of ether/ethanol=4/1 and dried to give 6-(2-chlorophenyl)-3-methyl-4-(1-methylguanidin-3-yl)imino-4,5,6,7-tetrahydroindazole hydrochloride (Compound 92) (80 mg) as colorless solid.

Provenance & Evidence