反应详情

To a mixture of 3,4-dihydro-2H-1-benzothiopyran (1.5 g) and 3-(1-acetylpiperidin-4-yl)propionyl chloride (2.18 g) in 1,2-dichloroethane (20ml) was added aluminum chloride (3.2 g) portionwise at 10°-15° C. The mixture was stirred at room temperature for 2 hours then refluxed for additional 2 hours, and poured into icewater. The mixture was extracted with dichloromethane, washed with water, dried over anhydrous sodium sulfate. The solvent was distilled off. The residue was purified by silica gel column chromatography (developing solvent: ethyl acetate) to obtain 2.7 g of the title compound as a pale yellow oil.

1. temperaturethen refluxed for additional 2 hours
2. additionpoured into icewater
3. extractionThe mixture was extracted with dichloromethane
4. washwashed with water
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off
7. customThe residue was purified by silica gel column chromatography (developing solvent: ethyl acetate)