反应详情

An ice cold solution of 3.63 g (14.3 mmol) of 15 in 60 mL of ether was treated with LiBH4 (621 mg, 28.5 mmol) and methanol (2 mL). After 30 min., 30 mL of 0.5 M NaOH solution was added. The mixture was extracted with ethyl acetate (2×25 mL) and the combined ethyl acetate solution washed with brine (50 mL), dried (MgSO4), filtered and evaporated. The residue was purified by flash chromatography on silica gel (5-20% ethyl acetate/hexane) to give 2.57 g (11.3 mmol, 79%) of the alcohol (16).

1. extractionThe mixture was extracted with ethyl acetate (2×25 mL)
2. washthe combined ethyl acetate solution washed with brine (50 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by flash chromatography on silica gel (5-20% ethyl acetate/hexane)