反应详情

A solution of the compound (200 mg, 0.458 mmol) obtained in Example 66, piperidine (210 μL, 2.29 mmol), N,N-dimethylaminopyridine (6 mg, 46 μmol), and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (264 mg, 1.37 mmol) in N,N-dimethylformamide (4.00 mL) was stirred at room temperature for 6 h. Saturated aqueous sodium hydrogencarbonate (100 mL) was added to the reaction mixture, the mixture was extracted with dichloromethane/2-propanol (4/1), and the organic layer was washed with water and dried with anhydrous sodium sulfate. Then the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:methanol=9:1 to 4:1) to obtain the title compound (26 mg, 11%) as a white solid.

1. extractionthe mixture was extracted with dichloromethane/2-propanol (4/1)
2. washthe organic layer was washed with water
3. dry with materialdried with anhydrous sodium sulfate
4. distillationThen the solvent was distilled off under reduced pressure
5. customThe residue was purified by silica gel column chromatography (ethyl acetate:methanol=9:1 to 4:1)