反应详情

To a solution of 4-(4-chloro-phenyl)-4-cyano-piperidine-1-carboxylic acid tert-butyl ester (500 mg, 1.56 mmol) in ethanol (15 ml) was added 2 ml 10 N aqueous sodium hydroxide. The resulting solution was warmed to reflux for 2 hours, cooled to room temperature, poured into 1 N aqueous hydrochloric acid, and extracted into ethyl acetate. The organic extracts were washed with brine, dried over magnesium sulfate, and concentrated in vacuo. Recovered yellow oil was purified by silica gel chromatography, eluting with dichloromethane-methanol (9.6:0.4) to give the title compound (306 mg, 58%). MS m/z: 339 (M+1)

1. temperatureThe resulting solution was warmed
2. temperatureto reflux for 2 hours
3. extractionextracted into ethyl acetate
4. washThe organic extracts were washed with brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customRecovered yellow oil
8. customwas purified by silica gel chromatography
9. washeluting with dichloromethane-methanol (9.6:0.4)