反应详情

A mixture of the product from Example 244C (56.2 mg, 0.259 mmol) and the product from Example 27A in acetic acid (1 mL) was heated under reflux for 2 h. The reaction mixture was cooled to room temperature and evaporated under reduced pressure. The resulting residue was triturated with methanol to provide the title compound (55.5 mg, 53% yield) as a beige solid. 1H NMR (300 MHz, DMSO-D6) δ ppm: 10.37 (s, 1H), 9.65 (s, 1H), 9.03 (s, 1H), 8.80 (s, 1H), 8.31 (s, 1H), 7.38 (d, J=8.09 Hz, 1H), 7.21 (d, J=8.82 Hz, 2H), 7.03 (dd, J=8.09, 1.47 Hz, 1H), 6.68 (d, J=8.82 Hz, 2H), 3.35-3.46 (m, 1H), 2.37 (s, 3H), 1.38 (d, J=6.62 Hz, 6H). MS (ESI+) m/z 404.2 (M+H)+ (ESI−) m/z 402.3 (M−H)−.

1. temperatureunder reflux for 2 h
2. customevaporated under reduced pressure
3. customThe resulting residue was triturated with methanol