反应详情

To a 3-necked flask is added 1′-methanesulfonyl-1′,2′,3′,6′-tetrahydro-[2,4′]bipyridinyl-5-ol (254.3 g, 1.0 mol) followed by 4-(1-methanesulfonyloxy-ethyl)-piperidine-1-carboxylic acid tert-butyl ester (396.1 g,1.34 mol) and potassium carbonate (248.8 g, 1.8 mol). Dimethylformamide (3800 mL) is added and the mixture is heated at 80˜90° C. for 6 h. 3810 mL of water are added dropwise at 70˜80° C. The mixture is cooled slowly to 20˜30° C. and filtered. The cake is slurried with 1000 mL of water, concentrated and dried under vacuum to provide 407 g of a solid with 97.13% HPLC purity.

1. temperaturethe mixture is heated at 80˜90° C. for 6 h
2. temperatureThe mixture is cooled slowly to 20˜30° C.
3. filtrationfiltered
4. concentrationconcentrated
5. customdried under vacuum