反应详情

To a suspension of the compound (100 mg) obtained in Example 157 in anhydrous tetrahydrofuran (THF; 20 ml) was added lithium borohydride (5.5 mg) under cooling with ice. The mixture was stirred for 5 minutes. After adding another lithium borohydride (5.5 mg), the mixture was stirred for further 5 minutes. Water was added to the reaction mixture, followed by extraction with methylene chloride. The organic layer was washed with saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/methylene chloride=1:1) to yield 45 mg (48%) of the titled compound.

1. temperatureunder cooling with ice
2. stirringthe mixture was stirred for further 5 minutes
3. extractionfollowed by extraction with methylene chloride
4. washThe organic layer was washed with saturated aqueous solution of sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. customthe residue was purified by silica gel column chromatography (ethyl acetate/methylene chloride=1:1)