反应详情

温度

-10 °C

5-chloro-4-methylpyridin-2-amine (30 g, 210 mmol) was dissolved in concentrated sulfuric acid (150 mL), and the solution was cooled to −10° C. Nitric acid (36 mL, 806 mmol) was added dropwise. The reaction mixture was stirred at 55° C. for 3 hours. The reaction mixture was poured into an ice/water mixture, and the pH was adjusted to 8 by addition of concentrated aqueous ammonium hydroxide (22%). The resulting suspension was filtered, and the solids were washed with water and dried under vacuum to provide the title compound (23 g, 123 mmol, 58.3% yield).

1. filtrationThe resulting suspension was filtered
2. washthe solids were washed with water
3. customdried under vacuum