[NH2:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([CH3:14])[C:8]([N+:15]([O-:17])=[O:16])=[CH:7][C:3]=1[C:4]([NH2:6])=O.P(Cl)(Cl)(Cl)=O.O>C(#N)C>[NH2:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([CH3:14])[C:8]([N+:15]([O-:17])=[O:16])=[CH:7][C:3]=1[C:4]#[N:6]To a mixture of 2-amino-4-methyl-3,5-dinitrobenzamide (7) (12.5 kg) in acetonitrile (78.4 kg) is added phosphorus oxychloride (14.8 kg) over a period of about 35 minutes. The mixture is then heated to reflux. After approximately 3.25 hours, the mixture is cooled to about 25° C. and added to water (245 kg). The vessel that formerly contained the reaction mixture is rinsed with acetonitrile (16 kg) and the rinse solution is also added to the aforementioned water quench solution. The quench solution is then cooled to about 5° C. over a period of about 2 hours. The quench solution is then filtered, the vessel that formerly contained the quench solution is rinsed with water (93 kg), and the rinse solution is passed through the product-containing filter. The product obtained is then dried in a vacuum tray drier, at a temperature of about 47° C. and a vacuum of about 12 torr, to provide 2-amino-4-methyl-3,5-dinitrobenzonitrile (5) (9.6 kg, 83.5% yield).
Wird geladen…
