反应详情

To the compound 54 (114 mg) in a methylene chloride (2 ml) solution, carbonyl diimidazole (45 mg) was added, and the mixture was stirred at room temperature for 45 minutes. The reaction solution was cooled to 0° C., then 28% ammonia aqueous solution (2 ml) was added, and the mixture was stirred at that temperature for 1 hour. The reaction solution was diluted with chloroform and the resultant mixture successively washed with water, 1M hydrochloric acid, and brine. The organic layer was dried over anhydrous sodium sulfate, then was concentrated. The residue was purified by flash column chromatography (silica gel, chloroform/ethyl acetate=7/3 to 1/2) to obtain the title compound (40 mg).

1. temperatureThe reaction solution was cooled to 0° C.
2. stirringthe mixture was stirred at that temperature for 1 hour
3. washthe resultant mixture successively washed with water, 1M hydrochloric acid, and brine
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. concentrationwas concentrated
6. customThe residue was purified by flash column chromatography (silica gel, chloroform/ethyl acetate=7/3 to 1/2)