反应详情

A solution of the compound (150 mg, 0.344 mmol) obtained in Example 66, dimethylamine hydrochloride (140 mg, 1.72 mmol), N,N-dimethylaminopyridine (4 mg, 34 μmol), and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (198 mg, 1.03 mmol) in N,N-dimethylformamide (3.00 mL) was stirred at room temperature for 1.5 h. Saturated aqueous sodium hydrogencarbonate (100 mL) was added to the reaction mixture, the mixture was extracted with dichloromethane, and the organic layer was washed with water and dried with anhydrous sodium sulfate. Then the solvent was distilled off under reduced pressure. Diisopropyl ether was added to the residue, and the precipitate was collected by filtration and dried under reduced pressure to obtain the title compound (153 mg, 96%) as a white solid.

1. extractionthe mixture was extracted with dichloromethane
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. additionDiisopropyl ether was added to the residue
6. filtrationthe precipitate was collected by filtration
7. customdried under reduced pressure