反应详情

A solution of 5-(2,6-difluorophenyl)-3-(6-(pyridin-3-yloxy)pyrazin-2-yl)-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole (74 mg, 0.15 mmol) and HCl (5-6 M in IPA, 3.0 mL, 15.2 mmol) in 4 mL of MeOH was heated at 80° C. for 90 min. The reaction was cooled to RT and concentrated. The residue was diluted with CH2Cl2 and saturated NaHCO3 (aq.) was added slowly. The mixture was extracted with CH2Cl2 (3×). The combined organic layers were dried over anhydrous Na2SO4, filtered and concentrated to give the title compound (55 mg, 0.14 mmol, 90% yield) as a yellow solid. MS (ESI, pos. ion) m/z: 402.0 (M+1). 1H NMR (400 MHz, DMSO-d6) δ ppm 13.77 (s, 1H), 9.15 (s, 1H), 8.60 (s, 1H), 8.56 (d, J=2.15 Hz, 1H), 7.99 (d, J=4.30 Hz, 1H), 7.82 (dd, J=8.22, 1.37 Hz, 1H), 7.69 (d, J=8.61 Hz, 1H), 7.53-7.62 (m, 1H), 7.49 (s, 1H), 7.37 (d, J=8.61 Hz, 1H), 7.25-7.33 (m, 2H), 7.23 (dd, J=8.41, 4.69 Hz, 1H).

1. concentrationconcentrated
2. additionThe residue was diluted with CH2Cl2 and saturated NaHCO3 (aq.)
3. additionwas added slowly
4. extractionThe mixture was extracted with CH2Cl2 (3×)
5. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated