反应详情

A solution consisting of 34.5 g (200 mmol) of 2-chloro-4-hydroxy-benzoic acid, 5 mL of concentrated sulfuric acid and 400 mL of ethanol was refluxed for 18 hours. 1.2 L of water were added to the resulting mixture followed by extraction with 1.5 L of methylene chloride. The mixture was then washed with aqueous sodium bicarbonate solution and water and dried with magnesium sulfate followed by distilling off the solvent. The residue was recrystallized from hexane/ethyl acetate to obtain 20.4 g of a light orange solid.

1. temperaturewas refluxed for 18 hours
2. extractionfollowed by extraction with 1.5 L of methylene chloride
3. washThe mixture was then washed with aqueous sodium bicarbonate solution and water
4. dry with materialdried with magnesium sulfate
5. distillationby distilling off the solvent
6. customThe residue was recrystallized from hexane/ethyl acetate