反应详情

To a solution of 4-[2-(4-glycoloylpiperazin-1-yl)-6-phenylpyrido[2,3-d]pyrimidin-7-yl]benzaldehyde (8-1) (136 mg, 0.292 mmol, prepared from 6-4 and 2-oxo-2-piperazin-1-ylethanol according to the procedure described for the synthesis of 7-1) in DM (5 mL) was added 2-(5-piperidin-4-yl-4H-1,2,4-triazol-3-yl)pyridine trifluoroacetate (73 mg, 0.32 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 oily residue was purified by reverse phase HPLC (Acetonitrile/0.1% TFA in water gradient) to afford the title compound. LRMS m/z (M+H) Calcd.: 667.8, found 667.5.

1. customdescribed for the synthesis of 7-1) in DM (5 mL)
2. washwashed with NaHCO3 (sat.)
3. dry with materialdried with MgSO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe oily residue was purified by reverse phase HPLC (Acetonitrile/0.1% TFA in water gradient)