反应详情

温度

110 °C

Perfluorophenyl 4-methoxy-2,6-dimethylbenzenesulfonate (1 g, 2.616 mmol), 2-(hydroxymethyl)-piperidine (1.61 g, 13.079 mmol) and tetrabutylammonium chloride (1.45 g, 5.231 mmol) were dissolved in N,N-dimethylformamide (10 ml) and the solution was stirred at 110° C. for 1 h. The solvent was removed in vacuo, the residue was dissolved in ethyl acetate and the solution was washed with ammonium chloride solution (10%, 20 ml), dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography (silica gel) with diethyl ether/hexane/methylene chloride (1:1:1). Yield: 0.63 g (76%)

1. customThe solvent was removed in vacuo
2. dissolutionthe residue was dissolved in ethyl acetate
3. washthe solution was washed with ammonium chloride solution (10%, 20 ml)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by column chromatography (silica gel) with diethyl ether/hexane/methylene chloride (1:1:1)