反应详情

A mixture of Example 20 (0.357 g, 0.656 mmol) and trifluoroacetic acid (0.506 mL, 6.56 mmol) in CH2Cl2 (6 mL) was stirred at room temperature for 6 hours. The reaction mixture was concentrated and purified by HPLC as described in Example 1F to provide the title compound as a trifluoroacetic acid salt. 1H NMR (300 MHz, CD3OD) δ ppm 3.14 (t, J=6.35 Hz, 2H), 3.54 (t, J=6.35 Hz, 2H), 4.43 (s, 2H), 7.07 (d, J=1.98 Hz, 1H), 7.31 (d, J=8.33 Hz, 1H), 7.52-7.63 (m, 3H), 7.66-7.72 (m, 2H), 7.76 (s, 1H), 7.87 (d, J=1.98 Hz, 1H), 9.18 (s, 1H). MS (ESI+) m/z 444.2 (M+H)+.

1. concentrationThe reaction mixture was concentrated
2. custompurified by HPLC