反应详情

4 g of sodium hydroxide was dissolved in 250 ml of water. Therein was dissolved 27.9 g of 3-methylsulfonylamino-4-phenoxyphenol. Thereto was added an aqueous solution obtained by dissolving 10.9 g of 3-chloropropionic acid and 4 g of sodium hydroxide in 30 ml of water. The mixture was refluxed for 30 minutes. The reaction mixture was water-cooled and adjusted to pH 8 with 4N hydrochloric acid. 70 ml of ethyl acetate was added thereto. The aqueous layer was separated, adjusted to pH 4 with 4N hydrochloric acid and extracted with 100 ml of ethyl acetate. The resulting extracts were washed with water and a saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue was mixed with diethyl ether. The resulting solid was collected by filtration to obtain 8.1 g (yield: 23.1%) of 3-(3-methylsulfonylamino-4-phenoxyphenoxy)propionic acid having a melting point of 145°-149° C.

1. additionThereto was added an aqueous solution
2. customobtained
3. temperatureThe mixture was refluxed for 30 minutes
4. temperaturecooled
5. customThe aqueous layer was separated
6. extractionextracted with 100 ml of ethyl acetate
7. washThe resulting extracts were washed with water
8. dry with materiala saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate
9. customThe solvent was removed by distillation under reduced pressure
10. additionThe residue was mixed with diethyl ether
11. filtrationThe resulting solid was collected by filtration