反应详情

A solution of 2-(4-fluorophenyl)-3-(methoxycarbonyl)pyridine-1-oxide (10.5 g.) in acetic anhydride (500 ml.) was stirred at reflux for 17 hr., cooled, evaporated to dryness and the residue partitioned between saturated sodium bicarbonate solution and ethyl acetate. The organic layer was separated, dried and evaporated to dryness. The gum obtained was dissolved in methanol (400 ml.), treated with a solution of potassium carbonate (11.7 g.) in water (100 ml) and stirred at ambient temperature for 2 hours. The methanol was evaporated off, the aqueous residue diluted with more water (200 ml.) and the mixture filtered to give methyl 2-(4-fluorophenyl)-6-hydroxypyridin-3-carboxylate (8.0 g.) as a brown solid.

1. temperatureat reflux for 17 hr
2. temperature, cooled
3. customevaporated to dryness
4. customthe residue partitioned between saturated sodium bicarbonate solution and ethyl acetate
5. customThe organic layer was separated
6. customdried
7. customevaporated to dryness
8. customThe gum obtained
9. customThe methanol was evaporated off
10. additionthe aqueous residue diluted with more water (200 ml.)
11. filtrationthe mixture filtered