反应详情

To a solution of 4-bromo-1-hydroxy-2-naphthoic acid (see Example 1, 1.63 g, 6.10 mmol) in 35 mL of acetone was added dimethyl sulfate (1.75 mL, 18.3 mmol) and potassium carbonate (2.95 g, 21.4 mmol). The reaction was heated to reflux for 14 hours, cooled to room temperature, filtered, and concentrated in vacuo. The residue was purified via silica gel chromatography, eluting with 0-20% ethyl acetate in hexanes to provide methyl 4-bromo-1-methoxy-2-naphthoate that gave a proton NMR spectra consistent with theory.

1. temperatureThe reaction was heated
2. temperatureto reflux for 14 hours
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe residue was purified via silica gel chromatography
6. washeluting with 0-20% ethyl acetate in hexanes