反应详情

温度

100 °C

A mixture of methyl-5,6-diaminonicotinate (461 mg, 2.76 mmol), formic acid (250 μL) and triethyl orthoformate (7.5 mL) was heated to 100° C. for 2 h. The mixture was then concentrated to an oily solid. Silica gel chromatography (8:1:1 EtOAc-MeOH—NH4OH) afforded the title compound as a cream-colored solid: Rf (8:1:1 EtOAc-MeOH—NH4OH)=0.22; 1H NMR (400 MHz, DMSO-d6): δ8.94 (d, J=2.0 Hz, 1H), 8.64 (s, 1H), 8.50 (d, J=2.0 Hz, 1H), 3.91 (s, 3H).

1. concentrationThe mixture was then concentrated to an oily solid