反应详情

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.

1. customcrystals precipitated during the reaction
2. filtrationwere filtered
3. washwashed with ethanol
4. additionTo the crystals were added ethyl acetate (60 ml) and 2 N sodium hydroxide (5 ml)
5. dissolutionto dissolve the crystals
6. washThe separated ethyl acetate layer was washed with water (10 ml, thrice), to which
7. additionwas added 2 N hydrochloric acid (0.3 ml)
8. concentrationThe mixture was concentrated under reduced pressure
9. washthe residue was washed with a mixture of ether/ethanol=4/1
10. customdried