反应详情

温度

160 °C

Compound 27 (1 g, 3.46 mmol) was added to formamide (1.167 mL, 29.3 mmol) and heated to 160° C. for 40 hours. Afterwards, the reaction mixture was allowed to cool to room temperature and diluted into ice cold water. The mixture was filtered and a solid was collected (943 mg, 91% yield): 1H NMR (400 MHz, DMSO) δ 12.37 (s, 1H), 9.32 (s, 1H), 8.81 (d, J=7.8, 1H), 8.23 (d, J=8.1, 1H), 8.13 (s, 1H), 7.75 (t, J=8.0, 1H), 5.06 (hept, J=6.6, 1H), 1.52 (d, J=6.7, 6H); 13C NMR (100 MHz, DMSO) δ 157.77, 152.48, 148.16, 148.06, 143.85, 133.58, 129.95, 123.05, 122.07, 103.02, 49.07, 21.74; [M+H]+ calculated for C14H13N5O3 300.1, found 300.0.

1. temperatureto cool to room temperature
2. additiondiluted into ice cold water
3. filtrationThe mixture was filtered
4. customa solid was collected (943 mg, 91% yield)