反应详情

Under argon atmosphere, a mixture of 7-bromo-N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (200 mg), 4-[N-ethyl-N-(2-propoxyethyl)amino]phenyl borate (290 mg) and potassium carbonate (266 mg) in toluene/ethanol/water (10/1/1 ml) was stirred at room temperature for 1 hour. To the mixture was added tetrakistriphenylphosphinepalladium (40 mg), and the mixture was refluxed for 8 hours, cooled, extracted with ethyl acetate, washed with saturated brine, dried with magnesium sulfate and was concentrated under reduced pressure. The residue was purified with silica gel column chromatography (ethanol/ethyl acetate=1:3) to give crystals, which were recrystallized from ethanol to give pale yellow crystals of 7-[4-[N-ethyl-N-(2-propoxyethyl)amino]phenyl]-N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (Compound 71) (89 mg).

1. temperaturethe mixture was refluxed for 8 hours
2. temperaturecooled
3. extractionextracted with ethyl acetate
4. washwashed with saturated brine
5. dry with materialdried with magnesium sulfate
6. concentrationwas concentrated under reduced pressure
7. customThe residue was purified with silica gel column chromatography (ethanol/ethyl acetate=1:3)
8. customto give crystals, which
9. customwere recrystallized from ethanol