反应详情

N,N-Dimethylformamide (270 kg), 5-bromo-2-methyl-3-nitropyridine (90.0 kg, 415 mol), and N,N-dimethylformamide dimethyl acetal (108.0 kg, 906.3 mol) were added to a 2000 L vessel at RT. The reaction mixture was stirred at RT for 30 minutes, then heated to 90±5° C. over a 3-hour period and maintained at this temperature for 4 hours. The mixture was subsequently cooled to 25±5° C. Water (945 kg) was added while keeping the temperature of the mixture at 25±5° C. After the addition of water, the reaction mixture was stirred for 2 hours. The solids were centrifuged to obtain wet product, which was slurried in isopropanol (207 kg) for 1 hour at 25±5° C. The solids were centrifuged again to obtain the title compound as a wet solid (105 kg, 92.5 wt % assay). The product was used in the next step without additional drying.

1. temperatureheated to 90±5° C. over a 3-hour period
2. temperaturemaintained at this temperature for 4 hours
3. temperatureThe mixture was subsequently cooled to 25±5° C
4. customat 25±5° C
5. stirringthe reaction mixture was stirred for 2 hours
6. customto obtain wet product, which