反应详情

A solution of 4-[2-(4-fluorophenyl)-6-trifluoromethylpyrazolo[1,5-a]pyridin-3-yl]-N-(3-(4-methoxybenzyloxy)propyl)-2-pyrimidinamine (2.1 g, 3.8 mmol) in 4N HCl/dioxane (5 mL) was stirred at room temperature for 4.5 h, then heated to reflux for 1 h. The mixture was cooled to room temperature, neutralized with saturated aqueous NaHCO3, and extracted with EtOAc. The EtOAc extracts were dried (MgSO4), filtered, and the solvent was evaporated. The residue was triturated with 2% EtOAc/hexanes to afford a solid which was collected by filtration and dried to give the title compound as a white solid, 1.31 g (80% yield). 1H NMR (acetone-d6) δ 9.20 (s, 1H), 8.73 (d, 1H, J=9.3 Hz), 8.15 (d, 1H, J=5.1 Hz), 7.77 (m, 2H), 7.64 (d, 1H, J=9.9 Hz), 7.34 (m, 2H), 6.50 (s, 1H), 6.40 (d, 1H, J=5.1 Hz), 3.60–3.70 (m, 4H), 1.88 (m, 2H). MS (+ve ion electrospray) 432 (95), (MH+).

1. temperatureheated
2. temperatureto reflux for 1 h
3. extractionextracted with EtOAc
4. dry with materialThe EtOAc extracts were dried (MgSO4)
5. filtrationfiltered
6. customthe solvent was evaporated
7. customThe residue was triturated with 2% EtOAc/hexanes
8. customto afford a solid which
9. filtrationwas collected by filtration
10. customdried