反应详情

To a solution of 0.14 mmol 4-cyanophenol in 1 ml N,N-dimethylformamide was added 0.19 mmol sodium hydride (60% suspension in oil) and the mixture was stirred at room temperature for 30 min. 0.12 mmol methanesulfonic acid 1-(2-isopropoxy-5-methanesulfonyl-benzoyl)-piperidin-4-yl ester was then added, and the reaction mixture was stirred at 60° C. for 2 h and then at 80° C. for 3 h. The reaction mixture was then cooled to room temperature and concentrated in vacuo. The crude material was purified by reversed phase HPLC (acetonitrile/water) to afford the title compound as a white crystalline solid (yield 21%). MS (m/e): 443.4 (M+H+, 100%).

1. stirringthe reaction mixture was stirred at 60° C. for 2 h
2. waitat 80° C. for 3 h
3. temperatureThe reaction mixture was then cooled to room temperature
4. concentrationconcentrated in vacuo
5. customThe crude material was purified by reversed phase HPLC (acetonitrile/water)