反应详情

温度

40 °C

1H-pyrazolo[3,4-b]pyridine-3-carbonitrile, as described in Step C of Example 158 (30 g, 208 mmol), 3-bromo-1,1,1-trifluoropropane (44.5 mL, 416 mmol) and potassium carbonate (95 g, 687 mmol) were combined in a flask with acetonitrile (300 mL) and stirred at 40° C. After 5 h, the reaction was cooled to rt and EtOAc and water were added. The layers were separated and the aqueous layer was washed two times with EtOAc. The combined organics were dried (Na2SO4) and filtered. The solvent was removed under reduced pressure and the material was used without further purification. 1H NMR (500 MHz, DMSO-d6): δ 8.77 (d, J=4.50 Hz, 1H); 8.46 (d, J=8.23 Hz, 1H); 7.51 (dd, J=8.22, 4.47 Hz, 1H); 4.86 (t, J=6.66 Hz, 2H); 3.10-2.98 (m, 2H). m/z=241.1 (M+H).

1. temperaturethe reaction was cooled to rt
2. customThe layers were separated
3. washthe aqueous layer was washed two times with EtOAc
4. dry with materialThe combined organics were dried (Na2SO4)
5. filtrationfiltered
6. customThe solvent was removed under reduced pressure
7. customthe material was used without further purification