反应详情

温度

50 °C

A mixture of 2-amino-5-(benzyloxy)-1-(biphenyl-3-yl)pyridin-4(1H)-one (2.65 g, 7.19 mmol) and 10% Pd/C (230 mg) in EtOH (300 mL) was stirred under an H2 balloon for 2 h. After this time, LCMS indicated that the reaction was complete. After evacuation and purge with N2 (3×), the EtOH solution was warmed to 50° C. and stirred 1 h at 50° C. The warmed EtOH solution was filtered and the catalyst was washed with warmed EtOH (4×50 mL). The combined EtOH solution was concentrated to give 2-amino-1-(biphenyl-3-yl)-5-hydroxypyridin-4(1H)-one as slightly yellow solid. 1H NMR (500 MHz, DMSO): δ 7.81 (d, J=7.9 Hz, 1 H); 7.76 (d, J=7.7 Hz, 2 H); 7.71-7.59 (m, 2 H); 7.49 (t, J=7.6 Hz, 2 H); 7.43-7.37 (m, 2 H); 6.91 (s, 1 H); 5.66 (s, 2 H); 5.54 (s, 1 H). HRMS Calcd for (C17H14N2O2+H)+ 279.1128. Found 279.1128.

1. customAfter evacuation and purge with N2 (3×)
2. stirringstirred 1 h at 50° C
3. filtrationThe warmed EtOH solution was filtered
4. washthe catalyst was washed with warmed EtOH (4×50 mL)
5. concentrationThe combined EtOH solution was concentrated