反应详情

To a solution of Intermediate 65 (0.298 g, 0.91 mmol) and Intermediate 3 (0.79 g, 0.70 mmol) in MeCN (2 mL) was added EDC (0.188 g, 0.98 mmol). The reaction mixture was stirred at room temperature for 18 hours. The reaction mixture was diluted with pyridine (2 mL) and heated at 150° C. under microwave irradiation for 20 minutes. The solvent was removed in vacuo and the residue dissolved in DCM. The mixture was washed with water and the organic phase passed through a hydrophobic frit. The solvent was evaporated in vacuo. The residue was purified by flash chromatography (silica, iso-hexane/EtOAc) to afford the title compound. 1H NMR (CDCl3, 400 MHz) δ 8.43 (1H, d, J=1.8 Hz), 8.17 (1H, dd, J=7.9, 1.9 Hz), 7.99 (1H, d, J=7.9 Hz), 7.59 (1H, s), 7.42 (1H, dd, J=8.0, 1.6 Hz), 7.37-7.21 (4H, m), 7.13 (1H, d, J=7.4 Hz), 4.22 (2H, m), 3.75 (2H, s), 3.31 (3H, s), 3.22 (2H, s), 2.41 (3H, s), 2.08 (3H, s), 1.50 (9H, s).

1. temperatureheated at 150° C. under microwave irradiation for 20 minutes
2. customThe solvent was removed in vacuo
3. dissolutionthe residue dissolved in DCM
4. washThe mixture was washed with water
5. customThe solvent was evaporated in vacuo
6. customThe residue was purified by flash chromatography (silica, iso-hexane/EtOAc)