反应详情

温度

70 °C

To a solution of N-(5-(3,3-difluoropiperidin-1-yl)-1-(2-((trimethylsilyl)methoxy)ethyl)-1H-pyrazol-4-yl)pyrazolo[1,5-a]pyrimidine-3-carboxamide (1.0 g, 2.1 mmol) in 50 mL of ethanol was added HCl (1.75 mL of a 6 M solution in water, 10.5 mmol). The reaction mixture was stirred at 70° C. for 1 hour. After cooling to room temperature, a light yellow precipitate formed, which was filtered off and rinsed with methanol and diethyl ether. The filtrate was then reduced in volume, and more solid product isolated by filteration. The combined collected solids were dried under vacuum to afford 0.77 g (94%) of N-(3-(3,3-difluoropiperidin-1-yl)-1H-pyrazol-4-yl)pyrazolo[1,5-a]pyrimidine-3-carboxamide. LCMS (ESI) m+H=348.1; 1H NMR (400 MHz, CDCl3) δ: 9.59 (s, 1H), 9.37 (dd, 1H), 8.84 (m, 2H), 8.01 (s, 1H), 7.32 (dd, 1H), 3.74 (s, 1H), 3.33 (m, 2H), 3.12 (m, 2H), 2.10 (m, 2H), 2.00 (m, 2H).

1. temperatureAfter cooling to room temperature
2. customa light yellow precipitate formed
3. filtrationwhich was filtered off
4. washrinsed with methanol and diethyl ether
5. customisolated by filteration
6. customThe combined collected solids
7. customwere dried under vacuum