反应详情

2-Amino-3-bromo-5-nitro-benzonitrile (1.9003 g, 7.85 mmol) was heated with urea (1.8862 g, 31.4 mmol) at 180–185° C. for 3 hrs. The cooled mixture was powered and treated with bicarbonate solution, filtered and washed with water. The solid was the collected and washed with ethanol, ether, and used for the next step reaction without further purification. 2.0 g product was obtained. Yield 89%; 1H NMR (500 MHz, DMSO-d6): δ 8.44455–8.45011(d, J=2.78 Hz, 1H), 8.87071–8.87544(d, J=2.365 Hz, 1H), 9.39866–9.40333(d, J=2.335 Hz, 1H), 9.50740–9.51282(d, J=2.71 Hz, 1H); ESI-MS: 285, 287 (M++1)

1. filtrationfiltered
2. washwashed with water
3. customcollected
4. washwashed with ethanol, ether
5. customused for the next step reaction without further purification