反应详情

To a solution of (R)-6-(4-chloro-3-cyclopropyl-1-methyl-1H-pyrazol-5-yl)-2-(3,5-dimethyl-1-tosyl-1H-indazol-4-yl)-4-(4-methoxy-3,3-dimethylpiperidin-1-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (0.050 g, 0.068 mmol) in MeOH (3 mL) was added K2CO3 (0.057 g, 0.410 mmol). The mixture was heated at 55C. under a nitrogen atmosphere for 2 h. At that point the mixture was diluted with EtOAc and washed with sat aq NH4Cl and then brine. The organic layer was dried over sodium sulfate, filtered and concentrated. The residue was purified by FCC (0-10% MeOH/DCM) to give the title compound. 1H NMR (400 MHz, DMSO-d6) δ ppm 12.59 (s, 1 H), 7.39 (d, J=8.3 Hz, 1 H), 7.21 (d, J=8.8 Hz, 1 H), 4.39 (d, J=14.9 Hz, 1 H), 4.25 (d, J=14.7 Hz, 1 H), 3.62-3.78 (m, 1 H), 3.56 (s, 3 H), 3.46-3.55 (m, 2 H), 3.30 (d, J=3.5 Hz, 1 H), 3.26 (s, 3 H), 2.99-3.08 (m, 1 H), 2.97 (dd, J=9.1, 4.0 Hz, 1 H), 2.92 (app. t, J=5.9 Hz, 2 H), 2.85 (d, J=12.9 Hz, 1 H), 2.18 (s, 3 H), 1.85-1.96 (m, 4 H), 1.74-1.82 (m, 1 H), 1.49-1.60 (m, 1 H), 0.92 (s, 3 H), (overlapped m, 2 H), 0.81 (s, 3H), 0.72-0.77 (m, 2 H); MS (ESI+) m/z 575.5 (M+H)+.

1. washwashed with sat aq NH4Cl
2. dry with materialThe organic layer was dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by FCC (0-10% MeOH/DCM)