反应详情

To a solution of 4B (206 mg, 0.550 nmol) in THF (5 mL) at −78° C. under nitrogen was added dropwise 1.0 M lithium triethylborohydride in tetrahydrofuran (3.00 mL, 3.00 mmol). The reaction was allowed to warm to rt and was stirred for 4 h. The reaction was quenched by pouring over ice (50 g) and stirring for 30 min. The product was extracted into EtOAc and washed with saturated aqueous NaHCO3 and brine. The organic layer was dried over MgSO4, filtered and concentrated. Purification via silica gel chromatography (0-15% EtOAc in hexane) provided the title compound (131 mg).

1. customThe reaction was quenched
2. additionby pouring over ice (50 g)
3. stirringstirring for 30 min
4. extractionThe product was extracted into EtOAc
5. washwashed with saturated aqueous NaHCO3 and brine
6. dry with materialThe organic layer was dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated
9. customPurification via silica gel chromatography (0-15% EtOAc in hexane)