反应详情

温度

160 °C

To a stirred suspension of N-(2-Amino-5-nitropyridin-3-yl)-4-nitrobenzamide (6) (1.15 g, 3.8 mmol) in ethylene glycol (75 mL) was added HCl (Conc., 3 drops) and the mixture heated at 160° C. for 6 h. The solution was cooled to room temperature and poured into H2O (200 mL) and the resulting solid collected by filtration, rinsed with H2O, and dried in vacuo at 80° C. to give 4 as a pale yellow solid (1 g, 3.5 mmol, 92%). 1H NMR (500 MHz, DMSO-d6) δ14.58 (br s, 1H), 9.28 (apparent d, 1H), 8.88 (br s, 1H), 8.51 (d, J=8.39 Hz, 2H), 8.45 (d, J=8.28 Hz, 2H). EIMS M−1 284.3. Rf=0.55 (silica, 19:1 DCM/MeOH)

1. temperatureThe solution was cooled to room temperature
2. filtrationthe resulting solid collected by filtration
3. washrinsed with H2O
4. customdried in vacuo at 80° C.