2,6-DICHLORO-3-NITRO-4-AMINOPYRIDINE

2587-03-3

2897-43-0

2,6-Dichloro-4-nitroaminopyridine (CAS: 2587-03-3, 1.66 g, 7.98 mmol) was used as a raw material, which was slowly added to 11 mL of concentrated sulfuric acid and stirred until completely dissolved. The reaction mixture was heated on a steam bath for 30 min. Upon completion of the reaction, the solution was cooled to room temperature and slowly poured into 28 g of crushed ice, which immediately formed a brown precipitate. The mixture was further cooled in an ice bath and the pH was adjusted dropwise to 7 by adding concentrated ammonium hydroxide solution.Subsequently, the reaction slurry was allowed to stand at -10 °C overnight. On the following day, the precipitate was collected by filtration through a Büchner funnel, washed thoroughly with pre-cooled deionized water and finally dried in a vacuum drying oven to afford the target product 4-amino-2,6-dichloro-3-nitropyridine (1.30 g, 78% yield) as a light tan solid.