反应详情

温度

100 °C

In 1,2-dimethoxyethane (15.3 ml) was dissolved methyl 7-(4-methyl-2-thienyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate. (510 mg), and to the solution was added 6N hydrochloric acid (10.2 ml). The mixture was stirred at 100° C. for 15 hours and cooled to room temperature. Under reduced pressure, the solvent was evaporated. To the residue,were added ethyl acetate and potassium carbonate solution, and the mixture was extracted with water. To the solution was added 6N hydrochloric acid, and the solution was made pH 4-5, extracted with ethyl acetate, washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated to give 7-(4-methyl-2-thienyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (459 mg).

1. temperaturecooled to room temperature
2. customUnder reduced pressure, the solvent was evaporated
3. additionTo the residue,were added ethyl acetate and potassium carbonate solution
4. extractionthe mixture was extracted with water
5. additionTo the solution was added 6N hydrochloric acid
6. extractionextracted with ethyl acetate
7. washwashed with saturated brine
8. dry with materialdried with magnesium sulfate
9. customUnder reduced pressure, the solvent was evaporated