反应详情

Methyl 4-(piperidin-2-yl)butanoic acid methyl ester hydrochloride (1.26 g, 5.683 mmol) was dissolved in dichloromethane (25 ml) and triethylamine (4 ml, 28.417 mmol) and a solution of 4-methoxy-2,6-dimethylbenzenesulfonic acid chloride (2.67 g, 11.37 mmol) in dichloromethane (10 ml) was added. The mixture was stirred overnight at room temperature. 1 mol/l HCl solution (10 ml) was added to the reaction mixture, followed by phase separation and extraction of the aqueous phase with dichloromethane (2×20 ml). The combined organic phases were washed with saturated sodium chloride solution (20 ml), dried over sodium sulfate and concentrated to small volume under vacuum. The crude product was purified by column chromatography (silica gel) with hexane/dichloromethane/diethyl ether (400:100:50). Yield: 1.65 g (75%)

1. customfollowed by phase separation and extraction of the aqueous phase with dichloromethane (2×20 ml)
2. washThe combined organic phases were washed with saturated sodium chloride solution (20 ml)
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated to small volume under vacuum
5. customThe crude product was purified by column chromatography (silica gel) with hexane/dichloromethane/diethyl ether (400:100:50)