反应详情

The resultant product (476 mg) of (1-5) and ethylamine hydrochloride (98 mg) were dissolved in dimethylformamide (2 mL), then 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (288 mg), hydroxybenzotriazole hydrate (230 mg) and triethylamine (167 μL) were added, and the mixture was stirred overnight at room temperature. A saturated aqueous sodium hydrogen carbonate solution was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography using a mixed solvent of chloroform and methanol as an eluent. The solvent was evaporated from the eluent to give the title compound (free form, 441 mg) as a pale-yellow amorphous solid. By a similar method as in (1-2), the title compound (357 mg) was obtained as pale-yellow crystals from the obtained residue.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe extract was washed with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. customthe solvent was evaporated under reduced pressure
5. customThe obtained residue was purified by silica gel column chromatography
6. customThe solvent was evaporated from the eluent