反应详情

To a solution of 4-(1-tert-butoxycarbonylpyrrolidin-3-yloxy)phenol (2.14 g) in tetrahydrofuran (43 l) were added ethyl bromoacetate (1.1 ml) and 60% sodium hydride (368 mg) with ice-cooling, and the mixture was stirred at room temperature for 1 hour. After completion of the reaction, ice water was added and the mixture was extracted with ethyl acetate and washed with 10% aqueous citric acid solution. The organic layer was dried over anhydrous magnesium sulfate and the solvent was evaporated. The obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=7:3) and dried under reduced pressure to give the title compound (2.605 g).

1. temperaturecooling
2. additionwas added
3. extractionthe mixture was extracted with ethyl acetate
4. washwashed with 10% aqueous citric acid solution
5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
6. customthe solvent was evaporated
7. customThe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=7:3)
8. customdried under reduced pressure