反应详情

温度

-30 °C

In methylene chloride (6 ml) was dissolved 7-(4-ethoxyphenyl)-N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-2,3-dihydro-1-benzothiepine-4-carboxamide (199 mg). To the mixture was added at −30° C. m-chloroperbenzoic acid (93 mg), and the mixture was stirred at −30° C. for 30 minutes and added to an aqueous solution of saturated sodium thiosulfate. To the mixture was added saturated sodium bicarbonate solution, and the mixture was extracted with ethyl acetate, washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column chromatography (ethyl acetate/methanol=3/1→2/1, 1% triethylamine) to give 7-(4-ethoxyphenyl)-N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-1-oxo-2,3-dihydro-1-benzothiepine-4-carboxamide (Compound 83) (28 mg).

1. extractionthe mixture was extracted with ethyl acetate
2. washwashed with saturated brine
3. dry with materialdried with magnesium sulfate
4. customUnder reduced pressure, the solvent was evaporated
5. customthe residue was purified with silica gel column chromatography (ethyl acetate/methanol=3/1→2/1, 1% triethylamine)