反应详情

7-Benzylamino-6-(4-phenylpiperidine-1-carbonyl)pyrazolo[1,5-a]pyrimidine-3-carboxylic acid (0.9 g, 1.9 mmol) obtained in step 5 was dissolved in DMF (15 mL), 1,1′-carbonyldiimidazole (1.2 g, 7.6 mmol) was added, and the mixture was stirred at room temperature for 2 hr. Methanesulfonamide (0.9 g, 9.5 mmol) and DBU (1.4 g, 9.5 mmol) were added to the reaction mixture, and the mixture was stirred at 60° C. for 1 hr. 10% Aqueous citric acid solution (5 mL) and water (60 mL) were added to the reaction mixture, and the mixture was stirred at room temperature for 1 hr. The precipitate was collected by filtration, washed with water (50 mL), and purified by silica gel column chromatography (chloroform/methanol=95/5) to give compound a-1 (0.8 g, 81%).

1. stirringthe mixture was stirred at 60° C. for 1 hr
2. stirringthe mixture was stirred at room temperature for 1 hr
3. filtrationThe precipitate was collected by filtration
4. washwashed with water (50 mL)
5. custompurified by silica gel column chromatography (chloroform/methanol=95/5)
6. customto give compound a-1 (0.8 g, 81%)