反应详情

温度

22.5 °C

A solution of 4-methyl-3,5-dinitrobenzonitrile (10.5 kg; preparation see U.S. Pat. No. 3,162,675), 4-amino-4H-1,2,4-triazole (17.0 kg) and dimethyl sulfoxide (68.6 kg) was dosed into a mixture of lithium tert-butoxide (12.2 kg) and dimethyl sulfoxide (106.6 kg) over about 50 min, while maintaining the temperature of each solution at 20-25° C. After aging at 20-25° C. for about 2 h, acetic acid (8.9 kg) was dosed into the reaction mixture at about 20° C. over about 10 min. The product was crystallized by dosing water (158 L) into the reaction mixture over about 1.5 h at about 20° C. The product slurry was cooled to 10-15° C. and held at this temperature for about 45 min. The resultant slurry was filtered, and washed with water (106 L). The wet cake obtained was dried in a vacuum tray dryer at about 50° C. and 30 Torr to provide 2-amino-4-methyl-3,5-dinitrobenzonitrile as an orange-brown solid.

1. custompreparation
2. customThe product was crystallized
3. customover about 1.5 h
4. customat about 20° C
5. temperatureThe product slurry was cooled to 10-15° C.
6. waitheld at this temperature for about 45 min
7. filtrationThe resultant slurry was filtered
8. washwashed with water (106 L)
9. customThe wet cake obtained
10. customwas dried in a vacuum tray dryer at about 50° C.