反应详情

Potassium hexamethyldisilazide (0.5 M in toluene, 285 mL, 0.143 mol) was added dropwise to a solution of (4) (39 g, 0.119 mol) in THF (240 mL) under nitrogen and stirred at room temperature for 1 hour. A solution of ethyl 3-bromopropionate (22.8 mL, 0.178 mol, 1.5 eq) in THF (45 mL) was added to the reaction mixture all at once. After stirring at room temperature for 4 hours, the reaction was quenched with saturated NH4Cl solution (20 mL). The organic solution was dried over MgSO4, and solvent is evaporated. The crude oil was purified by flashed chromatography (hexane-AcOEt/8:1) to give light yellow oil (48.03 g, 94.4% yield).

1. stirringAfter stirring at room temperature for 4 hours
2. customthe reaction was quenched with saturated NH4Cl solution (20 mL)
3. dry with materialThe organic solution was dried over MgSO4, and solvent
4. customis evaporated
5. customThe crude oil was purified