反应详情

2.3 g of 4-carboxy-1-(5-cyanopyrid-2-yl)-piperidine, 2.0 g of methyl 4-piperidylacetate hydrochloride, 4.8 g of 2-[(1H)-benzotriazol-1-yl]-1,1,3,3-tetramethyl-uronium tetrafluoroborate and 5 ml of triethylamine in 75 ml of dimethylformamide is stirred at ambient temperature for 16 hours. The solvent is removed under reduced pressure. The residue is diluted with water and the aqueous phase is extracted with ethyl acetate. The organic phase is washed with water and saturated saline solution and dried over sodium sulphate. The solvent is removed under reduced pressure and the residue is chromatographed over silica gel. Yield: 2.75 g (74% of theory), Melting point: 112°-115° C. Rf value: 0.40 (silica gel; methylene chloride/methanol=15:1)

1. customThe solvent is removed under reduced pressure
2. additionThe residue is diluted with water
3. extractionthe aqueous phase is extracted with ethyl acetate
4. washThe organic phase is washed with water and saturated saline solution
5. dry with materialdried over sodium sulphate
6. customThe solvent is removed under reduced pressure
7. customthe residue is chromatographed over silica gel