反应详情

温度

90 °C

A mixture of compound 344 and hydrochloric acid (1 N aqueous solution) (7 mL) was stirred at 90° C. for 17 h. After concentration, the residue was subjected to reverse phase preparative HPLC (acetonitrile/H2O containing 0.1% TFA each, 40 min from 10 to 30%). Lyophilization provided compound 346 (50 mg) as a yellow solid (TFA salt). 1H NMR (500 MHz, DMSO-d6) δ ppm 10.94 (1 H, br. s.), 9.55 (1 H, s), 9.33 (1 H, s), 8.65 (1 H, d, J=6.1 Hz), 8.53 (1 H, d, J=5.9 Hz), 8.23 (1 H, d, J=9.5 Hz), 7.60 (1 H, d, J=9.8 Hz), 5.34 (1 H, dq, J=8.9, 8.8 Hz), 4.16 (2 H, br. s.), 3.40 (8 H, br. s.), 2.33-2.44 (2 H, m), 1.92-2.18 (4 H, m), 1.62-1.81 (2 H, m). LCMS-ESI (POS), M/Z, M+1: Found 474.2.

1. concentrationAfter concentration
2. custom40 min