Nitric Acid → 2,6-Dichloro-4-nitropyridine

Participants

Reaction Steps

To a solution of 95% concentrated nitric acid (21 mL) and 98% concentrated sulfuric acid (50 mL) was added 2,6-dichloropyridine-N-oxide (12.8 g, 78 mmol). After the reaction was performed at 148° C. by stirring for 1 h, it was continued when the temperature was increased to 156° C. until no nitrogen dioxide was released. The reaction solution was cooled to room temperature, poured into 150 g ice water, and adjusted to pH=6 with ammonia water to precipitate a solid product. It was subjected to suction filtration. The resultant crude product was recrystallized with petroleum ether to afford 10 g yellow solid with a yield of 66.4%.

Provenance & Evidence