反应详情

A mixture of Example 56A (0.260 g, 0.516 mmol) and trifluoroacetic acid (0.397 mL, 5.16 mmol) in CH2Cl2 (5 mL) was stirred at 40° C. for 4 hours. The reaction mixture was concentrated and purified by HPLC (see protocol in Example 1F) to provide the title compound as a trifluoroacetic acid salt. The salt was treated with saturated aqueous NaHCO3 followed by filtration and drying to give a free base form of the title compound. 1H NMR (400 MHz, DMSO-d6) δ 3.96 (s, 2H), 7.09 (d, J=1.8 Hz, 1H), 7.38-7.23 (m, 2H), 7.66-7.52 (m, 3H), 7.76-7.69 (m, 1H), 7.96-7.91 (m, 3H), 9.16 (s, 1H), 10.73-10.68 (m, 1H). MS (ESI+) m/z 404.2 (M+H)+.

1. concentrationThe reaction mixture was concentrated
2. custompurified by HPLC (see protocol in Example 1F)