反应详情

2.94 g of 3-{3-(piperidinomethyl)phenoxy}propylamine was dissolved in 80 ml of dichloromethane, and stirred under cooling in an ice bath. 1.60 g of 2-(acetylthio)acetic acid and 2.26 g of EDC were added to this solution, and stirred at 0° C. for 30 minutes then at room temperature overnight. 100 ml of water and 50 ml of dichloromethane were added to the reaction solution, and extraction was carried out. The dichloromethane layer was washed twice with water, and dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, and the residue was purified by silica gel column chromatography using methanol:dichloromethane=1:15 as developing solvent to obtain the colorless oily N-[3-{3-(piperidinomethyl)phenoxy}propyl]-2-(acetylthio)acetamide. Yield: 2.23 g.

1. temperatureunder cooling in an ice bath
2. stirringstirred at 0° C. for 30 minutes
3. customat room temperature
4. customovernight
5. washThe dichloromethane layer was washed twice with water
6. dry with materialdried over anhydrous magnesium sulfate
7. customThe solvent was evaporated in vacuo
8. customthe residue was purified by silica gel column chromatography