反应详情

To a solution of 4-[2-(4-acetylpiperazin-1-yl)-6-phenylpyrido[2,3-d]pyrimidin-7-yl]benzaldehyde (3-2; 61 mg, 0.14 mmol) in DMF (5 mL) was added 2-(5-piperidin-4-yl-4H-1,2,4-triazol-3-yl)pyridine trifluoroacetate (58 mg, 0.17 mmol) followed by Et3N (80 μL, 0.51 mmol), AcOH (91 μL, 1.5 mmol) and sodium triacetoxyborohydride (59 mg, 0.28 mmol). The reaction mixture was allowed to stir for 12 hr then diluted with EtOAc and washed with NaHCO3 (sat.), dried with MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by silica gel chromatography (100% CH2Cl2 to 85% CH2Cl2/15% MeOH) to afford the title compound. LRMS m/z (M+H) Calcd.: 651.7, found 651.3.

1. washwashed with NaHCO3 (sat.)
2. dry with materialdried with MgSO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by silica gel chromatography (100% CH2Cl2 to 85% CH2Cl2/15% MeOH)