反应详情

温度

20 °C

A solution of 4-methyl-3,5-dinitrobenzamide (6) (15.1 kg) in dimethyl sulfoxide (95.6 kg) is added to a solution of 4-amino-1,2,4-triazole (21.6 kg) and potassium tert-butoxide (21.7 kg) in dimethyl sulfoxide (144.5 kg) at a rate to maintain a temperature of about 20° C. The mixture is allowed to stir for about 30 minutes, whereupon additional amounts of 4-amino-1,2,4-triazole (5.5 kg) and potassium tert-butoxide (3.7 kg) are added. The mixture is allowed to stir for about 1 hour at about 20° C., and then the mixture is added, over a period of about 30 minutes, to a cold (about 5° C.) solution of water (347 kg) and acetic acid (15 kg), allowing the temperature to rise to about 25° C. The vessel containing the initial reaction mixture is then rinsed with water (87 kg) and the rinse solution is also added to the acetic acid solution. The resulting mixture is cooled to about 5° C. and held at this temperature for about 30 minutes, whereupon the mixture is filtered and the solids obtained are washed with water (82 kg). The solids are then dried in a vacuum tray dryer for about 19 hours, at a temperature of about 50° C. and a vacuum of about 15 torr, to provide 2-amino-4-methyl-3,5-dinitrobenzamide (7) (13.6 kg, 84% yield).

1. additionare added
2. customto rise to about 25° C
3. additionThe vessel containing the initial
4. customreaction mixture
5. washis then rinsed with water (87 kg)
6. additionthe rinse solution is also added to the acetic acid solution
7. temperatureThe resulting mixture is cooled to about 5° C.
8. waitheld at this temperature for about 30 minutes, whereupon the mixture
9. filtrationis filtered
10. customthe solids obtained
11. washare washed with water (82 kg)
12. customThe solids are then dried in a vacuum tray dryer for about 19 hours, at a temperature of about 50° C.