反应详情

温度

60 °C

To a solution of 1.1 g of 1-(1,3-dioxolan-2-yl)methanamine in 10 mL of N,N-dimethylformamide, 1.6 mL of triethylamine and 2.0 g of 2-chloro-6-methoxy-3-nitropyridine were added at room temperature, and the mixture was stirred at 55 to 65° C. for 1 hour. The reaction mixture was cooled to room temperature, and ethyl acetate and water were then added thereto. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed sequentially with water and a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 2.7 g of N-(1,3-dioxolan-2-ylmethyl)-6-methoxy-3-nitropyridin-2-amine as a yellow solid.

1. temperatureThe reaction mixture was cooled to room temperature
2. customThe organic layer was separated
3. extractionthe aqueous layer was extracted with ethyl acetate
4. washthe resultant solution was washed sequentially with water
5. dry with materiala saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate
6. distillationthe solvent was distilled off under reduced pressure