反应详情

温度

22.5 °C

A solution of 4-methyl-3,5-dinitrobenzonitrile (4) (10.5 kg), 4-amino-1,2,4-triazole (17.0 kg) and dimethyl sulfoxide (68.6 kg) is dosed into a mixture of lithium t-butoxide (12.2 kg) and dimethyl sulfoxide (106.6 kg) over about 50 minutes, while maintaining the temperature of each solution at about 20-25° C. After aging at about 20-25° C. for about 2 hours, acetic acid (8.9 kg) is dosed into the reaction mixture at about 20° C. over about 10 minutes. The product is crystallized by dosing water (158 L) into the reaction mixture over about 1.5 hours at about 20° C. The product slurry is cooled to about 10-15° C. and held at this temperature for about 45 minutes. The resultant slurry is filtered, and washed with water (106 L). The wet cake obtained is dried in a vacuum tray dryer at about 50° C. and 30 torr until drying is complete to provide 2-amino-4-methyl-3,5-dinitrobenzonitrile (5) (9.8 kg, 87% Yield) as an orange-brown solid.

1. customThe product is crystallized
2. customover about 1.5 hours
3. customat about 20° C
4. temperatureThe product slurry is cooled to about 10-15° C.
5. waitheld at this temperature for about 45 minutes
6. filtrationThe resultant slurry is filtered
7. washwashed with water (106 L)
8. customThe wet cake obtained
9. customis dried in a vacuum tray dryer at about 50° C.
10. custom30 torr until drying