反应详情

温度

120 °C

(1-(4-Methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)methyl methanesulfonate (0.25 g, 0.639 mmol) and sodium iodide (0.383 g, 2.554 mmol) were dissolved in acetone (7 ml) and the solution was heated at 120° C. in a microwave oven (CEM Discover; 100 watt) for 1 h. The solvent was removed in vacuo, the residue was dissolved in sodium thiosulfate solution (20 ml, 5 mmol/l) and diethyl ether (40 ml), the phases were separated and the aqueous phase was extracted with diethyl ether (2×20 ml). The combined organic phases were dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography (silica gel) with hexane/diethyl ether/methylene chloride (3:1:1). Yield: 0.2 g (74%)

1. customThe solvent was removed in vacuo
2. dissolutionthe residue was dissolved in sodium thiosulfate solution (20 ml, 5 mmol/l)
3. customdiethyl ether (40 ml), the phases were separated
4. extractionthe aqueous phase was extracted with diethyl ether (2×20 ml)
5. dry with materialThe combined organic phases were dried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe crude product was purified by column chromatography (silica gel) with hexane/diethyl ether/methylene chloride (3:1:1)