反应详情

温度

100 °C

2-(2,2-Dimethoxy-ethyl)-6-(4-phenyl-butylcarbamoyl)-piperidine-1-carboxylic acid 9H-fluoren-9-ylmethyl ester (Compound 243, 1 g, 1.75 mmol) was dissolved in toluene (25 ml). Pyridinium p-toluene sulfonate (0.02 g, 0.08 mmol) was added and the reaction was stirred at 100° C. for 2 hours. After this time the reaction was cooled down, the toluene was evaporated and the residue was dissolved in EtOAc (75 mL), washed with saturated NaHCO3 solution (25 mL) and dried over Na2SO4. Flash chromatographic purification of the residue (1:2 EtOAc/hexanes) gave Compound 244 (0.770 g, 87%). Rf=0.5 (1:2 EtOAc/hexanes).

1. temperatureAfter this time the reaction was cooled down
2. customthe toluene was evaporated
3. dissolutionthe residue was dissolved in EtOAc (75 mL)
4. washwashed with saturated NaHCO3 solution (25 mL)
5. dry with materialdried over Na2SO4
6. customFlash chromatographic purification of the residue (1:2 EtOAc/hexanes)