反应详情

To a solution of Example 12D (40 mg, 0.077 mmol) in mixture of methanol/acetic acid (0.5 mL/0.5 mL), Zn powder (50 mg, 0.77 mmol) was added at room temperature. The reaction mixture was stirred for thirty minutes, filtered, concentrated under reduced pressure, and purified by high pressure liquid chromotography (eluting with 0-70% acetonitrile/water and 0.1% trifluoroacetic acid) to provide the title compound (25 mg, 66%). 1H NMR (400 MHz, methanol-d4) δ ppm 8.45 (s, 1H), 8.03 (s, 1H), 7.54 (s, 1H), 7.35-7.47 (m, 2H), 5.82 (m, 1H), 3.82-4.06 (m, 3H), 3.49-3.61 (m, 1H), 3.18 (s, 3H), 2.43-2.62 (m, 2H), 2.24-2.42 (m, 2H). MS (ESI) m/z 493 (M+H)+.

1. additionwas added at room temperature
2. filtrationfiltered
3. concentrationconcentrated under reduced pressure
4. custompurified by high pressure liquid chromotography (eluting with 0-70% acetonitrile/water and 0.1% trifluoroacetic acid)