反应详情

4-(2-Amino-ethyl)-1-(2-chloro-benzenesulfonyl)-piperidine-4-carboxylic acid ethyl ester (7.09 g) was suspended in toluene under an argon atmosphere, dimethylaluminium chloride in heptane (1 molar, 28.39 ml) was added and the mixture was stirred 5 minutes at RT then refluxed for 3 hours. It was then was cooled to RT, MeOH (40 ml) was added and the mixture was stirred for 30 minutes. The solvent was removed, the residue was adsorbed on silica gel and purified by flash chromatography over silica gel (eluents: AcOEt/CH2Cl2 5 to 50% then acetone/CH2Cl2 10 to 30%) to give the desired material (4.5 g) as light yellow solid. MS (ESI): 329.0 (MH+).

1. temperaturethen refluxed for 3 hours
2. temperatureIt was then was cooled to RT
3. stirringthe mixture was stirred for 30 minutes
4. customThe solvent was removed
5. custompurified by flash chromatography over silica gel (eluents