反应详情

To 5-methylsalicylic acid (3.04 g, 20 mmol) in DMF (100 ml) were added potassium carbonate (8.28 g, 60 mmol) and iodomethane (6.24 g, 44 mmol) under ice cooling and then the mixture was stirred at room temperature for 12 hours. The mixture were extracted by adding 5% sodium hydrogensulfite and ethyl acetate, and the extracted organic layer was washed with 5% citric acid and 5% brine. The organic layer was dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography (hexane-ethyl acetate) to give the captioned compound (3.43 g, 19.1 mmol, yield: 95%) as a colorless oil.

1. extractionThe mixture were extracted
2. additionby adding 5% sodium hydrogensulfite and ethyl acetate
3. washthe extracted organic layer was washed with 5% citric acid and 5% brine
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
5. concentrationconcentrated
6. customThe residue was purified by column chromatography (hexane-ethyl acetate)