反应详情

温度

80 °C

A mixture of 6-(5-isopropyl-2-methylphenyl)-4-methoxy-2-(5-methyl-1-tosyl-1H-indazol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (200 mg, 0.344 mmol), KOH (80 mg, 1.43 mmol) and concentrated aq NH4OH solution (4 mL) in MeOH (8 mL) was heated in a microwave reactor at 80° C. for 30 min. The reaction mixture was partitioned between EtOAc and water. The aqueous layer was extracted with EtOAc (3×). The combined organics were washed with brine, dried (Na2SO4) and concentrated. The residue was purified by silica gel chromatography (0-100% EtOAc/heptanes) to provide 6-(5-isopropyl-2-methylphenyl)-4-methoxy-2-(5-methyl-1H-indazol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine as a white solid. 1H NMR (400 MHz, CD2Cl2) δ ppm 8.31 (s, 1 H) 7.52 (d, J=8.34 Hz, 1 H) 7.40 (d, J=8.59 Hz, 1 H) 7.21 (d, J=7.83 Hz, 1 H) 7.11 (d, J=1.52 Hz, 1 H) 6.97 (dd, J=7.71, 1.64 Hz, 1 H) 4.04-4.20 (m, 5 H) 3.37 (t, J=5.68 Hz, 2 H) 3.19 (t, J=5.56 Hz, 2 H) 2.88-3.01 (m, 1 H) 2.70 (s, 3 H) 2.37 (s, 3 H) 1.31 (d, J=6.82 Hz, 6 H); MS (ESI+) m/z 428.1 (M+H)+.

1. customThe reaction mixture was partitioned between EtOAc and water
2. extractionThe aqueous layer was extracted with EtOAc (3×)
3. washThe combined organics were washed with brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated
6. customThe residue was purified by silica gel chromatography (0-100% EtOAc/heptanes)