反应详情

To a mixture 0.30 g (7.55 mmole) of sodium hydride (60% in mineral oil) and 30 mL of methanol was added 1.49 g (6.86 mmole) of 2,5-difluoro-4-nitro-benzoic acid methyl ester. The mixture was heated at reflux for 18 hours and then quenched by the addition of water, and then concentrated under reduced pressure. The residue was diluted with ethyl acetate, washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography eluting with dichloromethane-hexanes (1:1) to give 0.92 g of 2-fluoro-5-methoxy-4-nitro-benzoic acid methyl ester.

1. temperatureThe mixture was heated
2. temperatureat reflux for 18 hours
3. customquenched by the addition of water
4. concentrationconcentrated under reduced pressure
5. additionThe residue was diluted with ethyl acetate
6. washwashed with brine
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customThe residue was purified by silica gel chromatography
11. washeluting with dichloromethane-hexanes (1:1)