反应详情

3-(acetylamino)-4-methylbenzoic acid (300 g, 1.55 mol) was added portionwise to fuming nitric acid (1200 mL) with stirring over a period of 1 h at 0˜5° C. The solution gradually turned into a heavy slurry during the addition. At the end of addition, an additional fuming nitric acid (200 mL) was added. The reaction mixture was stirred for an additional hour at 5° C., then allowed to warm to room temperature and poured into ice water. The solid formed was collected and washed with water (450 mL×3). The crude product was re-crystallized from acetic acid (1800 mL) to give the title compound (191.5 g, 51.8%) as a white solid.

1. additionThe solution gradually turned into a heavy slurry during the addition
2. additionAt the end of addition
3. stirringThe reaction mixture was stirred for an additional hour at 5° C.
4. customThe solid formed
5. customwas collected
6. washwashed with water (450 mL×3)
7. customThe crude product was re-crystallized from acetic acid (1800 mL)