反应详情

Under an argon atmosphere, to a solution of 2.79 g of 5-(benzyloxy)-2-(methoxycarbonyl)-3,4-dihydronaphthalene in 30 ml of dry dichloromethane, 24 ml of diisobutylaluminum hydride (1M toluene solution) was added dropwise at −70° C. or lower, followed by stirring for 20 minutes. To the reaction solution, 26 ml of an aqueous 10% sodium hydroxide solution was added dropwise and, after heating to room temperature, the mixture was extracted with diethyl ether. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 2.25 g of the desired compound as a colorless crystal having a melting point of 59 to 61° C.

1. extractionthe mixture was extracted with diethyl ether
2. washThe extract was washed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customthe solvent was evaporated under reduced pressure
5. customThe residue was purified by silica gel column chromatography