反应详情

6-(7-Hydroxy-6,7-dihydro-5H-pyrrolo[1,2-c]imidazol-7-yl)-N-methyl-2-naphthamide (77 mg) was dissolved in methanol (5 ml). 1 N Hydrochloric acid (0.5 ml) and 10% palladium carbon (50% wet, 39 mg) were added, and the mixture was vigorously stirred for 12 h under 4 kg/cm2 hydrogen atmosphere. The catalyst was filtered off and the residue was washed with methanol. The filtrate and the washing were combined and aqueous potassium carbonate solution (0.25 M; 1 ml) was added. After neutralization, the solvent was evaporated under reduced pressure, and the residue was purified by flash silica gel column chromatography (eluent, chloroform/methanol containing ammonia (7%); 19/1). The eluate was recrystallized from chloroform-ether to give the title compound (53 mg) as colorless crystals.

1. filtrationThe catalyst was filtered off
2. washthe residue was washed with methanol
3. additionaqueous potassium carbonate solution (0.25 M; 1 ml) was added
4. customAfter neutralization, the solvent was evaporated under reduced pressure
5. customthe residue was purified by flash silica gel column chromatography (eluent, chloroform/methanol containing ammonia (7%); 19/1)
6. customThe eluate was recrystallized from chloroform-ether