反应详情

Under argon atmosphere, a mixture of methyl 7-bromo-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (1.0 g), 4-fluorophenyl borate (0.465 g) and potassium carbonate (0.84 g) in toluene/ethanol/water (30/3/3 ml) was stirred at room temperature for 1 hour. To the mixture was added tetrakistriphenylphosphinepalladium (0.17 g), and the mixture was refluxed for 20 hours, cooled, extracted with ethyl acetate, saturated brine, dried with magnesium sulfate and concentrated under reduced pressure. The residue was purified with column chromatography (ethyl acetate/hexane=1:1) and recrystallized from ethyl acetate/hexane=1:1 to give pale yellow crystals of methyl 7-(4-fluorophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (656.3 mg).

1. temperaturethe mixture was refluxed for 20 hours
2. temperaturecooled
3. extractionextracted with ethyl acetate, saturated brine
4. dry with materialdried with magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified with column chromatography (ethyl acetate/hexane=1:1)
7. customrecrystallized from ethyl acetate/hexane=1:1