反应详情

To a solution of 4 (4.8 g, 12 mmol) in THF (100 mL) is added slowly 1 M DIBAL in toluene, (50 mL, 50 mmol) at −78° C. The mixture is stirred at room temperature for 1 hour and quenched with 20 mL of water. The solvent is evaporated, the residue is diluted with 100 mL of 1:1 saturated Rochells salt/15% NaOH, and this extracted with EtOAc (4×50 mL). The organic extracts are combined, dried and concentrated under vacuum. The residue is purified by flash chromatography (silica gel; Hexane/EtOAc 1:9) to provide 2.3 g (48%) of the title compound. M+H+=385.26.

1. customquenched with 20 mL of water
2. customThe solvent is evaporated
3. additionthe residue is diluted with 100 mL of 1:1 saturated Rochells salt/15% NaOH
4. extractionthis extracted with EtOAc (4×50 mL)
5. customdried
6. concentrationconcentrated under vacuum
7. customThe residue is purified by flash chromatography (silica gel; Hexane/EtOAc 1:9)