反应详情

3-Acetamido-4-methylbenzoic acid (205 g, 1061 mmol) was added portionwise over 45 min to stirred fuming nitric acid (1 L) at −5° C., maintaining a reaction temperature below 0° C. The mixture was stirred for an additional 1 h and then crushed ice (2.5 kg) was added. The mixture was stirred for a further 30 min. The precipite that formed was filtered off and thoroughly washed with water. The resulting cake was air dried and suspended in 1 L of acetic acid at 65° C. The suspension was stirred for 1 hour, allowed to cool down to RT and then filtered. The filtrate was washed with acetic acid and ether to give 3-acetamido-4-methyl-2-nitrobenzoic acid (160 g, 63%) as a white solid. MS (M+H)+ 239.

1. temperaturemaintaining a reaction temperature below 0° C
2. stirringThe mixture was stirred for a further 30 min
3. customThe precipite that formed
4. filtrationwas filtered off
5. washthoroughly washed with water
6. customdried
7. customsuspended in 1 L of acetic acid at 65° C
8. stirringThe suspension was stirred for 1 hour
9. filtrationfiltered
10. washThe filtrate was washed with acetic acid and ether