反应详情

温度

75 °C

To a solution of 6.6 g of sodium hydroxide in 60 ml of water at 5° C. was added 9.3 g of bromine. When a clear solution was obtained, 9.2 g of 3-aminocarbonyl-2-chloro-6-methyl-4-(trifluoromethyl)pyridine was added quickly, maintaining the temperature below 5° C. The resulting mixture was stirred until the 3-(aminocarbonyl)pyridine dissolved (~30 min). The cooling bath was removed and the mixture was then warmed to 75° C. for 30 min. After cooling to room temperature, the 3-aminopyridine product was extracted with ethyl acetate, dried (magnesium sulfate), filtered, and evaporated to give 4.9 g of the desired product.

1. customWhen a clear solution was obtained
2. temperaturemaintaining the temperature below 5° C
3. dissolutiondissolved (~30 min)
4. customThe cooling bath was removed
5. temperatureAfter cooling to room temperature
6. extractionthe 3-aminopyridine product was extracted with ethyl acetate
7. dry with materialdried (magnesium sulfate)
8. filtrationfiltered
9. customevaporated