反应详情

温度

70 °C

The product from Example 44B (0.035 g, 0.091 mmol) and 4 M hydrogen chloride in dioxane (0.023 mL, 0.091 mmol) were combined and heated at 70° C. for 24 hours, cooled and concentrated. Purification by reverse phase chromatography (C18, CH3CN/water (0.1% TFA), 10-100%) afforded the title compound (0.024 g, 53%) as the TFA salt. 1H NMR (300 MHz, DMSO-d6) δ ppm 10.95 (d, J=5.43 Hz, 1H) 7.62 (dd, J=8.82, 2.37 Hz, 1H) 7.45-7.48 (m, 2H) 6.86-6.91 (m, 1H) 6.84 (d, J=8.82 Hz, 1H) 6.21 (dd, J=6.78, 1.02 Hz, 1H) 5.50 (s, 1H) 4.12 (s, 3H) 3.09 (s, 3H) 3.05 (d, J=6.44 Hz, 2H) 0.95-1.14 (m, 1H) 0.38-0.45 (m, 2H) 0.17-0.24 (m, 2H). MS (ESI+) m/z 372 (M+H)+.

1. temperaturecooled
2. concentrationconcentrated
3. customPurification by reverse phase chromatography (C18, CH3CN/water (0.1% TFA), 10-100%)