反应详情

A mixture of the product of part (v) (0.50 g), 2-chloro-4-nitropyridine (0.28 g) and sodium bicarbonate (1.00 g) in n-butanol (20 ml) was heated under reflux with stirring for 18 hours. The mixture was cooled, filtered, and the residue was washed with ethanol. The combined filtrate and washings were evaporated to give a gum which was chromatographed on silica gel eluting with ether. Earlier fractions gave impurity and the pure product was eluted in the later fractions. The product fractions were combined and evaporated to give the product, (0.21 g), m.p. 183.5°-184.5° (from ethanol).

1. temperaturewas heated
2. temperatureunder reflux
3. temperatureThe mixture was cooled
4. filtrationfiltered
5. washthe residue was washed with ethanol
6. customThe combined filtrate and washings were evaporated
7. customto give a gum which
8. customwas chromatographed on silica gel eluting with ether
9. customEarlier fractions gave impurity
10. washthe pure product was eluted in the later fractions
11. customevaporated
12. customto give the product, (0.21 g), m.p. 183.5°-184.5° (from ethanol)