反应详情

Under argon atmosphere, a mixture of methyl 7-bromo-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (0.80 g), 4-ethoxyphenyl borate (0.44 g) and potassium carbonate (0.67 g) in toluene/ethanol/water (20/2/2 ml) was stirred at room temperature for 1 hour. To the mixture was added tetrakistriphenylphosphinepalladium (0.14 g), and the mixture was refluxed for 16 hours, cooled, extracted with ethyl acetate, washed with saturated brine, dried with magnesium sulfate and concentrated under reduced pressure. The resulting solid was recrystallized from ethyl acetate/hexane to give pale yellow crystals of methyl 7-(4-ethoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (739.5 mg).

1. temperaturethe mixture was refluxed for 16 hours
2. temperaturecooled
3. extractionextracted with ethyl acetate
4. washwashed with saturated brine
5. dry with materialdried with magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe resulting solid was recrystallized from ethyl acetate/hexane