反应详情

温度

60 °C

2-[3-(3-Aminopropoxy)benzylamino]-1-(β-D-ribofuranosyl)-1H-benzimidazole (0.2 g) and N-(benzyloxycarbonyl)-1H-pyrazol-1-carboxamidine (0.55 g) were suspended in tetrahydrofuran (2.5 mL), and the mixture was stirred at 60° C. for 24 hours. The reaction mixture was concentrated under reduced pressure, and the obtained residue was dissolved in methanol (4 mL). To the solution was added a catalytic amount of 10% palladium-carbon powder, and the mixture was stirred at 40° C. under a hydrogen atmosphere for 2 hour. The insoluble material was removed by filtration, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by preparative reverse phase column chromatography (Shiseido CAPSELL PAC C18UG80, 5 μm, 20×50 mm, flow rate 30 mL/minutes linear gradient, water/methanol=70/30-10/90) to give the title compound (0.01 g).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. dissolutionthe obtained residue was dissolved in methanol (4 mL)
3. additionTo the solution was added a catalytic amount of 10% palladium-carbon powder
4. stirringthe mixture was stirred at 40° C. under a hydrogen atmosphere for 2 hour
5. customThe insoluble material was removed by filtration
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe obtained residue was purified by preparative reverse phase column chromatography (Shiseido CAPSELL PAC C18UG80, 5 μm, 20×50 mm, flow rate 30 mL/minutes linear gradient, water/methanol=70/30-10/90)