反应详情

温度

60 °C

Into a solution of methyl 7-[[4-(propoxymethyl)benzyl]oxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (1.15 g) in THF/methanol (10/5 ml) was added at room temperature an aqueous solution (2.1 ml) of potassium carbonate (622 mg), and the resulting mixture was stirred at 60° C. for 2 days. After cooling to room temperature, the reaction mixture was extracted with ethyl acetate. To the aqueous layer was added 1 N hydrochloric acid until the pH was adjusted to 2-3, and the resulting mixture 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 diisopropyl ether to obtain 7-[[4-(propoxymethyl)benzyl]oxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (425 mg) as colorless crystals.

1. temperatureAfter cooling to room temperature
2. extractionthe reaction mixture was extracted with ethyl acetate
3. additionTo the aqueous layer was added 1 N hydrochloric acid until the pH
4. extractionthe resulting mixture was extracted with ethyl acetate
5. washThe organic layer was washed with an aqueous saturated solution of sodium chloride
6. dry with materialwas dried with magnesium sulfate
7. concentrationAfter concentration under reduced pressure
8. filtrationthe precipitated crystals were collected by filtration
9. washThe crystals were washed with diisopropyl ether