反应详情

温度

80 °C

To a solution of tert-butyl 6-fluoro-1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboxylate (2.55 g, 7.14 mmol) in NMP (30 mL) was added 4-methoxybenzylamine (2.80 mL, 21.41 mmol). The resulting mixture was then heated to 80° C. for 2 hours, after which the mixture was diluted with water (200 mL) and extracted with EtOAc (2×200 mL). The combined extracts were washed with water (100 mL), dried with MgSO4, filtered, absorbed onto silica gel (17 g) and removed the solvent in vacuo. This solid was purified on silica gel (80 g) column (0-100% EtOAc/CH2Cl2 to give the title compound. LRMS (M+1)=474.0

1. extractionextracted with EtOAc (2×200 mL)
2. washThe combined extracts were washed with water (100 mL)
3. dry with materialdried with MgSO4
4. filtrationfiltered
5. customabsorbed onto silica gel (17 g)
6. customremoved the solvent in vacuo
7. customThis solid was purified on silica gel (80 g) column (0-100% EtOAc/CH2Cl2