反应详情

温度

80 °C

Phosphorus oxychloride (91.3 kg) is added over about 30 minutes into a mixture of 4-methyl-3,5-dinitrobenzamide (6) (66.6 kg) in acetonitrile (250.2 kg). The mixture is heated at reflux (about 80° C.) for about 2.5 hours. The solution is then cooled to ambient temperature and added to water (335 L) over about 1.5 hour, while maintaining a temperature of less than about 30° C. The mixture is cooled to about 5° C. and held at this temperature for about 18 hours. The product that precipitates is isolated via centrifugation, washed with water (469 L), and dried in a convection tray dryer at about 45° C. for about 22 hours to provide 4-methyl-3,5-dinitrobenzonitrile (4) (59 kg, 96% yield).

1. temperatureThe mixture is heated
2. temperatureThe solution is then cooled to ambient temperature
3. temperaturewhile maintaining a temperature of less than about 30° C
4. temperatureThe mixture is cooled to about 5° C.
5. customThe product that precipitates
6. customis isolated via centrifugation
7. washwashed with water (469 L)
8. customdried in a convection tray dryer at about 45° C. for about 22 hours