反应详情

Ethyl {[2-(1,3-benzodioxol-5-yl)-2-oxoethyl]thio}acetate (Method 11) (15.8 g, 0.056 mol) was dissolved in benzene (500 mL) and 2,2-dimethyl-1,3-propanediol (46.6 g, 0.45 mol) and p-toluene sulfonic acid (cat., 500 mg) were added. The mixture was stirred at reflux in a Dean-Stark apparatus for two hours, given room temperature and concentrated under reduced pressure. The resulting white solid was dissolved in CH2Cl2 (500 mL) and washed twice with water (300 mL) and brine (300 mL). The organic layer was dried (MgSO4) and concentrated under reduced pressure. The crude oil was purified by flash-chromatography (heptane:EtOAc 4:1) to afford the desired product.

1. temperatureat reflux in a Dean-Stark apparatus for two hours
2. customgiven room temperature
3. concentrationconcentrated under reduced pressure
4. dissolutionThe resulting white solid was dissolved in CH2Cl2 (500 mL)
5. washwashed twice with water (300 mL) and brine (300 mL)
6. dry with materialThe organic layer was dried (MgSO4)
7. concentrationconcentrated under reduced pressure
8. customThe crude oil was purified by flash-chromatography (heptane:EtOAc 4:1)