反应详情

To a solution of 2-hydroxymethyl-6-methylpyridine (Example 67 part b, 0.5 g), in anhydrous dimethylformamide (20 ml) under nitrogen was added sodium hydride (107 mg of 60% in oil) and the reaction mixture was stirred at room temperature for 0.5 hours. To this mixture was added 6-chloro-3-phenyl-1,2,4-triazolo[3,4-a]phthalazine (Example 67 part d, 330 mg) and the solution was heated to 80° C. for 0.25 hours. After cooling the solvent was removed under vacuum, and the residue was dissolved in dichloromethane (30 ml) and washed with water and brine. After drying (MgSO4), the solution was filtered and evaporated to give the required product which was recrystallised from a mixture of ethyl acetate and hexane to give the title compound (210 mg, m.p. 186-187° C.). 1H NMR (360 MHz, DMSO) δ 2.52 (3H, s), 5.65 (2H, s), 7.25 (1H, d, J=7.7Hz), 7.49 (1H, d, J=7.7Hz), 7.58 (3H, m), 7.76 (1H, t, J=7.7Hz), 7.94 (1H, t, J=7.6Hz), 8.08 (1H, t, J=7.7Hz), 8.30 (3H, m), 8.58 (1H, d, J=7.6Hz); MS (ES+) m/e 368 [MH]+. Anal. Found C, 71.32; H, 4.44; N. 18.53. C22H17N5O. H2O requires C, 71.22; H, 4.73; N, 18.88%.

1. temperaturethe solution was heated to 80° C. for 0.25 hours
2. temperatureAfter cooling the solvent
3. customwas removed under vacuum
4. dissolutionthe residue was dissolved in dichloromethane (30 ml)
5. washwashed with water and brine
6. dry with materialAfter drying (MgSO4)
7. filtrationthe solution was filtered
8. customevaporated