反应详情

温度

5 °C

To a 1900 ml of concentrated sulfuric acid 630 g of 6-diethylamino-2-picoline were dropwise added while cooling with ice water. A 70% nitric acid solution of 347 g were dropwise added at not more than 5° C. over about 2 hours to the resulting mixture and stirred at 5° C. for additional one hour. The reation mixture was added to 4 kg of ice, neutralized with a sodium hydroxide solution, and extracted two times with ethyl acetate. The extract solution was washed two times with water, dried over anhydrous magnesium sulfate, concentrated and dried. Thus, 775 g of 6-diethylamino-3-nitro-2-picoline were obtained.

1. extractionextracted two times with ethyl acetate
2. washThe extract solution was washed two times with water
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated
5. customdried