反应详情

To a stirred solution of 1-(4-bromophenyl)piperidine-4-carboxylic acid (1.56 g, 5.5 mmol) in absolute ethanol (30 mL) was cooled to 0° C. and SOCl2 (1.18 g, 10 mmol) added drop-wise. The mixture was stirred to room temperature and heated to reflux for 3 hours. The reaction mixture was evaporated in vacuo and the residue dissolved in saturated aqueous solution of NaHCO3 (50 mL). The aqueous solution was extracted with EtOAc (3×30 mL). The organic extracts was dried over Na2SO4, filtered and evaporated in vacuo. The residue was purified by silica gel column chromatography (eluent; ethyl acetate: hexane=1:1) to yield the title compound pale brown oil 1.08 g. MS (m/z): 314 (M+2)+

1. temperatureheated
2. temperatureto reflux for 3 hours
3. customThe reaction mixture was evaporated in vacuo
4. dissolutionthe residue dissolved in saturated aqueous solution of NaHCO3 (50 mL)
5. extractionThe aqueous solution was extracted with EtOAc (3×30 mL)
6. dry with materialThe organic extracts was dried over Na2SO4
7. filtrationfiltered
8. customevaporated in vacuo
9. customThe residue was purified by silica gel column chromatography (eluent; ethyl acetate: hexane=1:1)