反应详情

To a solution of step D product, 3-f, (1.2 g, 2.8 mmol) in MeOH (100 mL) was added Pd/C (200 mg, 10%) and HCO2NH4 (0.36 g, 5.6 mmol). The mixture was stirred and refluxed for 5 h. The reaction mixture was filtered. The liquids were concentrated and purified by column chromatography to afford the product, 3-g (590 mg, 64%). 1H NMR (300 MHz, DMSO) δ 4.30 (d, J=4.2 Hz, 2H), 5.66 (s, 1H), 7.21-7.35 (m, 11H), 8.66 (s, 1H), 9.64 (s, 1H). LC-MS (M+H)+ 326.1.

1. temperaturerefluxed for 5 h
2. filtrationThe reaction mixture was filtered
3. concentrationThe liquids were concentrated
4. custompurified by column chromatography