反应详情

To a stirring solution of the ester 46.4 (1.5 g, 6.9 mmol) in anhydrous THF (40 mL) is added dropwise a solution of LiAlH4 in THF (1.0 M, 13.7 mL, 13.7 mmol) at 0° C. The mixture is stirred until TLC confirms the consumption of the starting material. The reaction is slowly quenched with water (10 mL) at 0° C., 1N NaOH aqueous solution (50 mL) and another portion of water (10 mL). The mixture is filtered and the filtrate is extracted with EtOAc (3×100 mL), dried over MgSO4 and concentrated in vacuo. The residue is purified by column chromatography (silica, EtOAc/Hexane), to afford alcohol 46.5.

1. customthe consumption of the starting material
2. customThe reaction is slowly quenched with water (10 mL) at 0° C.
3. filtrationThe mixture is filtered
4. extractionthe filtrate is extracted with EtOAc (3×100 mL)
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. customThe residue is purified by column chromatography (silica, EtOAc/Hexane)