反应详情

温度

70 °C

The product from Example 45A (0.12 g, 0.30 mmol) and 4 M hydrogen chloride in dioxane (5 mL, 20.00 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 (0.068 g, 45%) as the TFA salt. 1H NMR (300 MHz, DMSO-d6) δ ppm 10.91 (d, J=5.09 Hz, 1H) 7.70 (dd, J=8.48, 2.37 Hz, 1H) 7.61 (d, J=2.37 Hz, 1H) 7.54-7.56 (m, 1H) 7.21 (d, J=8.48 Hz, 1H) 6.84 (dd, J=7.12, 5.76 Hz, 1H) 6.31 (d, J=5.76 Hz, 1H) 4.11 (s, 3H) 3.15 (s, 3H) 2.77 (s, 3H) 2.74 (d, J=6.78 Hz, 2H) 0.64-0.78 (m, 1H) 0.28-0.37 (m, 2H) −0.11-−0.05 (m, 2H). MS (ESI+) m/z 386 (M+H)+.

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