反应详情

1-[(1,1-Dimethylethoxycarbonyl)amino]-piperidine-4-carboxylic acid (6 g, 26.16 mmol, 1 eq.), from step 1, was dissolved in methanol (150 ml) and cesium carbonate (4.26 g, 13.08 mmol, 0.5 eq.) was added. The mixture was stirred at room temperature for 2 h, the solvent was removed under reduced pressure. The crude was dissolved in DMF (100 ml) and benzylbromide (5.37 g, 31.39 mmol, 1.2 eq.) was added dropwise. The mixture was stirred overnight at room temperature and poured in water (300 ml), extracted with Ethyl Acetate (900 ml) The organic layer was dried over anhydrous sodium sulfate and evaporated under reduced pressure to give a white solid. Yield 95%, 7 g.

1. customthe solvent was removed under reduced pressure
2. dissolutionThe crude was dissolved in DMF (100 ml)
3. stirringThe mixture was stirred overnight at room temperature
4. extractionextracted with Ethyl Acetate (900 ml) The organic layer
5. dry with materialwas dried over anhydrous sodium sulfate
6. customevaporated under reduced pressure
7. customto give a white solid