反应详情

A suspension mixture of 4-amino-2,6-dichloronicotinamide (1.12 g, 6.53 mmol) and triethyl orthoformate (20 mL, 17.8 g, 120.3 mmol) was heated at 150° C. for 6 hours in a Teflon screwed pressure vessel. After it was cooled to room temperature, evaporation of triethyl orthoformate afforded crude product that was crystallized from a mixed solvent of toluene and methanol to afford product the title compound. 1H NMR (DMSO-d6) 7.55 (d, J=5.6 Hz, 1H), 8.30 (s, 1H), 8.55 (d, J=5.6 Hz, 1H), 12.72 (br s, 1H, NH); 13C NMR (DMSO-d6) δ 116.4, 121.0, 149.9, 150.9, 151.4, 157.6, 158.0; ESI-MS m/z 181.0 (MH+).

1. customevaporation of triethyl orthoformate
2. customafforded crude product that
3. customwas crystallized from a mixed solvent of toluene and methanol