反应详情

To a solution of 1.50 g of 1-(4-ethoxycarbonyl-2-fluorophenyl)piperidine-4-carboxamide in 20 ml of THF, 2.0 ml of triethylamine and 0.9 ml of trifluoroacetic acid anhydride were added at −78° C., and the mixture was stirred at room temperature for 6 hours. The solvent was evaporated, EtOAc was added, and then the organic layer was washed with water and brine, and dried over sodium sulfate. After the evaporation of the solvent, the residue was purified by silica gel column chromatography (eluent:hexane-EtOAc=5:1˜4:1) to obtain 1.43 g of 4-(4-cyanopiperidino)-3-fluorobenzoic acid ethyl ester.

1. customThe solvent was evaporated
2. additionEtOAc was added
3. washthe organic layer was washed with water and brine
4. dry with materialdried over sodium sulfate
5. customAfter the evaporation of the solvent
6. customthe residue was purified by silica gel column chromatography (eluent:hexane-EtOAc=5:1˜4:1)