反应详情

To 0.5 g (3.4 mmol) 4-phenyl-2-azetidinone in 5 mL anhydrous THF under nitrogen was added a solution of lithium aluminium hydride (1 M in THF, 11.9 mmol) dropwise, and the mixture was heated at reflux for 4 hours. The reaction mixture was cooled to room temperature, 20% aqueous ammonium chloride was added and the mixture was filtered through a pad of celite. The filtrate was extracted with EtOAc (2×10 mL), the organic layers were combined and dried over Na2SO4. After filtration and evaporation of the solvent the product was purified by column chromatography (silica, DCM/7 N ammonia in MeOH 92:2 to 94:6), which was used in the next step without further purification.

1. temperaturethe mixture was heated
2. temperatureat reflux for 4 hours
3. filtrationthe mixture was filtered through a pad of celite
4. extractionThe filtrate was extracted with EtOAc (2×10 mL)
5. dry with materialdried over Na2SO4
6. filtrationAfter filtration and evaporation of the solvent the product
7. customwas purified by column chromatography (silica, DCM/7 N ammonia in MeOH 92:2 to 94:6), which
8. customwas used in the next step without further purification