反应详情

温度

0 °C

157.6 g (1 mole) of 2-chloro-6-ethoxy-pyridine were slowly added over 45 minutes with stirring to a mixture of 190 ml of concentrated sulfuric acid, 190 ml of 24% oleum and 100 ml of 97% nitric acid while keeping the reaction temperature between 20° and 40° C. with cooling and the mixture was allowed to stand for 5 hours while the temperature returned to room temperature. The mixture was cooled to 0° C. and filtered with a glass frit filter. The solid product was suspended in a mixture of 100 g of potassium carbonate and 250 ml of water and the suspension was stirred for 3 hours at 30° C. and was vacuum filtered. The product was washed with water and dried at 40° C. to obtain 192 g (93% yield) of 2-chloro-3-nitro-6-ethoxy-pyridine with a purity of 98%.

1. customthe reaction temperature between 20° and 40° C.
2. temperaturewith cooling
3. customreturned to room temperature
4. filtrationfiltered with a glass frit
5. filtrationfilter
6. additionThe solid product was suspended in a mixture of 100 g of potassium carbonate and 250 ml of water
7. filtrationfiltered
8. washThe product was washed with water
9. customdried at 40° C.