反应详情

温度

80 °C

While cooling a mixture of 3-ethyl-2-methylpyridine 1-oxide (7.35 g, 53.6 mmol) and sulfuric acid (22.7 g, 231 mmol) in an ice bath, fuming nitric acid (3.64 ml, 87.9 mmol) was added dropwise, which was stirred at 80° C. for 8 hours. The reaction mixture was cooled to room temperature and then poured into ice. The obtained aqueous solution was extracted three times with chloroform. The organic layers were combined, dried over anhydrous magnesium sulfate, filtrated and concentrated to obtain the title compound (3.37 g, yield: 34.5%) as yellow solid.

1. temperatureWhile cooling
2. additionwas added dropwise
3. temperatureThe reaction mixture was cooled to room temperature
4. additionpoured into ice
5. extractionThe obtained aqueous solution was extracted three times with chloroform
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltrated
8. concentrationconcentrated