反应详情

10 g of concentrated sulfuric acid was added to a methanol (120 g) solution of 50 g of 3,5-dichlorobenzoic acid, and the mixture was refluxed by heating for 5 hours. After cooling the reaction solution to room temperature, the solvent was distilled off under reduced pressure. The obtained residue was dissolved into 200 g of ethyl acetate, washed with water (200 g×2), then washed with a saturated aqueous solution of sodium bicarbonate, and further washed with water. After drying the organic phase over anhydrous magnesium sulfate, 48.6 g of the target product was obtained as a white solid by removing the solvent by distilling under reduced pressure.

1. temperaturethe mixture was refluxed
2. temperatureby heating for 5 hours
3. distillationthe solvent was distilled off under reduced pressure
4. dissolutionThe obtained residue was dissolved into 200 g of ethyl acetate
5. washwashed with water (200 g×2)
6. washwashed with a saturated aqueous solution of sodium bicarbonate
7. washfurther washed with water
8. dry with materialAfter drying the organic phase over anhydrous magnesium sulfate