反应详情

温度

0 °C

Compound 12 (2.64 g, 8.16 mmol) was dissolved in toluene (40 mL), and diisobutylaluminum hydride (1.0 mol/L toluene solution, 24.5 mL) was added to the solution at 0° C. under argon atmosphere, followed by stirring at 0° C. for 1.5 hours. The reaction mixture was added with a saturated aqueous (+)-potassium sodium tartrate tetrahydrate solution to terminate the reaction, and diluted with ethyl acetate, followed by stirring vigorously for 30 minutes. The organic layer was separated from the aqueous layer, and washed with saturated brine, and dried over anhydrous magnesium sulfate, then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=5:1) to obtain Compound 13 (2.32 g, yield 90%).

1. customto terminate
2. customthe reaction
3. stirringby stirring vigorously for 30 minutes
4. customThe organic layer was separated from the aqueous layer
5. washwashed with saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=5:1)