反应详情

温度

110 °C

Methyl 4-fluoro-2-hydroxybenzoate (3.00 g), 5-chloro-2-nitropyridine (3.08 g), and potassium carbonate (4.87 g) were added to dimethyl sulfoxide (50 mL), heated to 110° C. for one hour, cooled, added to water, and extracted with ethyl ether. The ether was washed with brine and dried on anhydrous sodium sulfate. The solution was filtered and concentrated and purified by flash column chromatography on silica gel using 10% ethyl acetate in hexanes increasing to 20% ethyl acetate in hexanes and increasing again to 30% ethyl acetate in hexanes.

1. temperaturecooled
2. extractionextracted with ethyl ether
3. washThe ether was washed with brine
4. dry with materialdried on anhydrous sodium sulfate
5. filtrationThe solution was filtered
6. concentrationconcentrated
7. custompurified by flash column chromatography on silica gel using 10% ethyl acetate in hexanes increasing to 20% ethyl acetate in hexanes
8. temperatureincreasing again to 30% ethyl acetate in hexanes