反应详情

温度

155 °C

4-Chloro-6-(1H-indazol-4-yl)-1-methyl-1H-pyrazolo[3,4-b]pyridine 7 (0.1 g, 0.352 m moles) was dissolved in 2 mL DMF. 4-Methylsulfonylphenol 8a (0.12 g, 0.704 mmol) and potassium carbonate (0.24 g, 1.76 mmol) were added. After bubbling nitrogen gas through the reaction mixture, it was heated by microwave at 155° C. for 1.5-2 hours. Solvent was removed, excess potassium carbonate was filtered and partitioned and extracted with ethyl acetate. The organic portions were washed with saturated sodium bicarbonate solution followed by brine, dried over anhydrous Na2SO4, solvent removed and purified to obtain 101. 1H NMR (400 MHz, DMSO) δ 13.26 (s, 1H), 8.77 (s, 1H), 8.06 (d, J=8.8, 2H), 7.92-7.51 (m, 6H), 7.51-7.27 (m, 2H), 4.13 (s, 3H), 3.28 (s, 3H) MS (ESI) m/z 420.1 (M+1)+

1. customAfter bubbling nitrogen gas through the reaction mixture, it
2. customSolvent was removed
3. filtrationexcess potassium carbonate was filtered
4. custompartitioned
5. extractionextracted with ethyl acetate
6. washThe organic portions were washed with saturated sodium bicarbonate solution
7. dry with materialdried over anhydrous Na2SO4, solvent
8. customremoved
9. custompurified