反应详情

The compound (900 mg) obtained in Example 58 was dissolved in N,N-dimethylformamide (50 ml), to which dimethylamine hydrochloride (304 mg), 1-hydroxybenzotriazole monohydrate (262 mg), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (369 mg) and diisopropylethylamine (1.83 ml) were added, and the mixture was stirred at room temperature for 12 hours. The solvent was distilled off under reduced pressure, and a saturated aqueous solution of sodium hydrogencarbonate was added to the residue to conduct extraction with methylene chloride. The resultant organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the resultant residue was purified by column chromatography on silica gel (methylene chloride:methanol=47:3). The thus-obtained white solids were dissolved in methylene chloride, to which 1N ethanol solution (1.49 ml) of hydrochloric acid was added. The solvent was distilled off under reduced pressure, and methanol and diethyl ether were added to the residue to collect precipitate formed by filtration, thereby obtaining the title compound (777 mg).

1. additionwere added
2. distillationThe solvent was distilled off under reduced pressure
3. additiona saturated aqueous solution of sodium hydrogencarbonate was added to the residue
4. extractionextraction with methylene chloride
5. dry with materialThe resultant organic layer was dried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. customthe resultant residue was purified by column chromatography on silica gel (methylene chloride:methanol=47:3)
8. dissolutionThe thus-obtained white solids were dissolved in methylene chloride, to which 1N ethanol solution (1.49 ml) of hydrochloric acid
9. additionwas added
10. distillationThe solvent was distilled off under reduced pressure, and methanol and diethyl ether
11. additionwere added to the residue
12. customto collect precipitate
13. customformed by filtration