反应详情

A mixture of 5-formylsalicylic acid (4.98 g, 30 mmol), benzyl bromide (15.39 g, 90 mmol), potassium carbonate (16.59 g, 120 mmol), and methyl ethyl ketone (350 mL) was refluxed for 8 hours. After cooling, the solvent was evaporated under reduced pressure. 2N Hydrochloric acid was added to the residue, and the mixture was extracted with ethyl acetate. The layer was washed with water and brine, and dried over anhydrous magnesium sulfate. The residue obtained by evaporation of the solvent under reduced pressure was purified by column chromatography on silica gel (n-hexane:ethyl acetate=3:1), suspended and washed with isopropyl ether under heating at reflux to give the title compound (5.98 g, 57.5%) as a white solid.

1. temperaturewas refluxed for 8 hours
2. temperatureAfter cooling
3. customthe solvent was evaporated under reduced pressure
4. addition2N Hydrochloric acid was added to the residue
5. extractionthe mixture was extracted with ethyl acetate
6. washThe layer was washed with water and brine
7. dry with materialdried over anhydrous magnesium sulfate
8. customThe residue obtained by evaporation of the solvent under reduced pressure
9. customwas purified by column chromatography on silica gel (n-hexane:ethyl acetate=3:1)
10. washwashed with isopropyl ether
11. temperatureunder heating
12. temperatureat reflux