反应详情

温度

65 °C

Into a solution of methyl 7-[3-ethoxy-4-(2-propoxyethoxy)phenoxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (0.45 g) in THF-methanol (10-5 ml) was added at room temperature a 1 M aqueous solution of potassium carbonate (1.8 ml), and the resulting mixture was stirred at 65° C. for 20 hours. After cooling to room temperature, 1 N hydrochloric acid (10 ml) was added to the reaction mixture, which was extracted with ethyl acetate. The organic layer was washed with an aqueous saturated solution of sodium chloride and was dried with magnesium sulfate. After concentration under reduced pressure, the precipitated crystals were collected by filtration. The crystals were washed with hexane to obtain 7-[3-ethoxy-4-(2-propoxyethoxy)phenoxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (283 mg) as light yellow crystals.

1. temperatureAfter cooling to room temperature
2. extractionwas extracted with ethyl acetate
3. washThe organic layer was washed with an aqueous saturated solution of sodium chloride
4. dry with materialwas dried with magnesium sulfate
5. concentrationAfter concentration under reduced pressure
6. filtrationthe precipitated crystals were collected by filtration
7. washThe crystals were washed with hexane