反应详情

温度

100 °C

To a mixture of 165 mL of nitric acid and 209 mL of sulfuric acid was slowly added 56.4 g of 2-chloro-5-methylpyridine-1-oxide. The reaction mixture was stirred at 100° C. for two hours, cooled to room temperature, and added to ice. Sodium carbonate was added to adjust the pH to about pH 2 to pH 3. The resulting yellow solid was separated by filtration and washed with ice-water. The combined filtrates were extracted with hot chloroform. The extracts were combined, dried over sodium sulfate, and concentrated to give 59.1 g of 2-chloro-5-methyl-4-nitropyridine-1-oxide (80%). Mass Spec. M+H=189.

1. temperaturecooled to room temperature
2. additionadded to ice
3. customThe resulting yellow solid was separated by filtration
4. washwashed with ice-water
5. extractionThe combined filtrates were extracted with hot chloroform
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated