Water → 4-Methyl-3,5-dinitrobenzamide

Participants

Reaction Conditions

Reaction Steps

A mixture of 4-methyl-3,5-dinitrobenzoic acid (48.2 kg) (3) and sulfamide (50.1 kg) in pyridine (197 kg) is heated to reflux (about 115-120° C.) for about 1.5 hours. The solution is then cooled to ambient temperature and water is added (178 kg) over about 1 hour. The mixture is then cooled to about ˜5° C. and held at this temperature for about 1 hour. The product slurry is centrifuged and the solids obtained are washed with water (621 L). The product is dried in a vacuum tray dryer at a temperature of about 65° C. and a vacuum of about 10 torr to provide 4-methyl-3,5-dinitrobenzamide (6) (43.8 kg, 91.3% yield).

Provenance & Evidence