反应详情

To 2.26 g of tert-butyl 2-{5-(ethoxycarbonyl)-2-furylmethyl}-3-oxobutanoate in 50 ml of tetrahydrofuran, 7.7 ml of 1M lithium tri-sec-butylborohydride in tetrahydrofuran solution was added at -78° C. under stirring, and the resulting reaction solution was stirred at the same temperature for 2 hours. After addition of water, the reaction solution was stirred at room temperature for 30 minutes and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate. The desiccant was filtered off, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography [hexane/ethyl acetate=12/1→4/1] to give 1.65 g of the title compound.

1. customthe resulting reaction solution
2. stirringwas stirred at the same temperature for 2 hours
3. stirringthe reaction solution was stirred at room temperature for 30 minutes
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with saturated aqueous sodium chloride
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationThe desiccant was filtered off
8. distillationthe solvent was distilled off under reduced pressure
9. customThe residue was purified by silica gel column chromatography [hexane/ethyl acetate=12/1→4/1]