反应详情

温度

0 °C

Fuming nitric acid (120 mL, 2.8 mol) is cooled to about 0° C., whereupon 3-(Formylamino)-6-bromo-4-methylbenzoic Acid (20) (28.243 g, 109.5 mmol) is added in small portions over about 45 minutes, at such a rate to maintain the internal reaction temperature <5° C. The reaction mixture is then stirred at about 0° C. for about 1 hour. The reaction mixture is added to ice water (500 mL) and stirred for about 1 hour. The solids that form are filtered and dried to provide 3-(Formylamino)-6-bromo-4-methyl-2-nitrobenzoic Acid (21), as a beige powder (31.465 g, 95% yield).

1. additionis added in small portions over about 45 minutes
2. temperatureat such a rate to maintain the internal reaction temperature <5° C
3. stirringstirred for about 1 hour
4. filtrationThe solids that form are filtered
5. customdried