反应详情

To a solution of [6-(4-tert-butyl-cyclohexyloxy)-naphthalen-2-yl]-acetic acid ethyl ester (250 mg, 0.68 mmol) in THF (10 mL) was added 1.0 M of lithium tetrahydroaluminate in THF (2 mL, 2 mmol) at 0° C. After stirred at room temperature for 2 hrs, the solution was quenched with ethyl acetate (1 mL), then added Rochelle's salt aqueous (1.5 mL). The solution was stirred for 1 hr, then extracted with ethyl acetate. The organic phase was dried over MgSO4, filtered and concentrated. The resulting crude was purified via a silica gel column eluted with EtOAc in hexanes from 0 to 60% to give white precipitate (0.17 g, yield: 77%). ESI-MS: 327.20 (M+H)+.

1. customthe solution was quenched with ethyl acetate (1 mL)
2. stirringThe solution was stirred for 1 hr
3. extractionextracted with ethyl acetate
4. dry with materialThe organic phase was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe resulting crude was purified via a silica gel column
8. washeluted with EtOAc in hexanes from 0 to 60%