26820-34-8

85216-54-2

26820-34-8

General procedure for the synthesis of 2-chloro-6-methyl-5-nitropyridine-3-carbonitrile from 2-hydroxy-6-methyl-5-nitronicotinonitrile: Phosphoryl chloride (64 mL, 689 mmol) was slowly added to 6-dimethyl-5-nitro-2-oxo-1,2-dihydropyridine-3-carbonitrile (19.5 g, 107 mmol). Subsequently, phosphorus pentachloride (20.81 g, 100 mmol) was added to the reaction system. The reaction mixture was heated to 100 °C and the reaction was continuously stirred at this temperature for 20 hours. Upon completion of the reaction, the mixture was cooled to room temperature and quenched by careful pouring into an ice-water mixture. The precipitated solid product was collected by filtration, washed well with water and dried under appropriate conditions to afford the target compound 2-chloro-6-methyl-5-nitropyridine-3-carbonitrile. The yield was 80%. The product was characterized by 1H NMR (300 MHz, DMSO-d6): δ 10.45 (s, 1H), 2.77 (s, 3H); mass spectrum (ES): m/z 198.1 (M + 1).