反应详情

3-Ethoxy-2-methylpyridine (132.5 g) was added dropwise to concentrated sulphuric acid (530 ml) with stirring and cooling to keep the mixture below 10° C. A mixture of concentrated nitric acid (81 ml) and concentrated sulphuric acid (97 ml) was added dropwise over 4 hours, keeping the temperature below 5° C. The reaction mixture was allowed to warm up slowly to ambient temperature and then added in portions to ice/water (2.5 l). The solid was collected by filtration, washed with water and dried under vacuum at 50° C. to give 3-ethoxy-2-methyl-6-nitropyridine, m.p. 82°-84° C.

1. temperaturecooling
2. customthe mixture below 10° C
3. additionwas added dropwise over 4 hours
4. customthe temperature below 5° C
5. filtrationThe solid was collected by filtration
6. washwashed with water
7. customdried under vacuum at 50° C.