反应详情

The compound (6.29 g, 25.75 mmol) obtained in step A was dissolved in N-methylpyrrolidone (100 ml), and the mixture was stirred under ice-cooling. Thereto was added 60% sodium hydride (1.21 g, 30 mmol) and the mixture was stirred at room temperature for 20 min. After stirring, N-(3-bromopropyl)phthalimide (8.31 g, 31.0 mmol) was added and the mixture was stirred at 70° C. for 90 min. The reaction mixture was diluted with ethyl acetate, washed with water, saturated aqueous sodium hydrogen carbonate and saturated brine, and dried over anhydrous magnesium sulfate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure. The obtained solid was washed with diethyl ether-hexane mixed solvent, and dried under reduced pressure to give the title compound (8.11 g, yield 73%) as a colorless solid.

1. temperaturecooling
2. stirringthe mixture was stirred at room temperature for 20 min
3. stirringAfter stirring
4. stirringthe mixture was stirred at 70° C. for 90 min
5. washwashed with water, saturated aqueous sodium hydrogen carbonate and saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationThe insoluble material was filtered off
8. concentrationthe solution was concentrated under reduced pressure
9. washThe obtained solid was washed with diethyl ether-hexane mixed solvent
10. customdried under reduced pressure