反应详情

[4-(4-Nitrophenoxy)pyridin-2-yl]carbamic acid phenyl ester (100 mg) was dissolved in tetrahydrofuran (2 ml) under a nitrogen atmosphere, and then 4-(piperidin-1-yl)piperidine (144 mg) was added thereto, followed by stirring for 30 min. The reaction mixture was partitioned between ethyl acetate and a saturated aqueous solution of ammonium chloride. The organic layer was washed with a saturated aqueous solution of ammonium chloride, water and brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated under a reduced pressure to give a residue, which was then purified by silica gel column chromatography (Fuji Silysia NH, eluent; hexane:ethyl acetate=1:2 to 1:8). The solvent was evaporated under a reduced pressure to give a residue, which was then dried in vacuum to provide 4-(piperidin-1-yl)piperidine-1-carboxylic acid [4-(4-nitrophenoxy)pyridin-2-yl]amide as a crude product.

1. customThe reaction mixture was partitioned between ethyl acetate
2. washThe organic layer was washed with a saturated aqueous solution of ammonium chloride, water and brine in this order
3. dry with materialdried over anhydrous sodium sulfate
4. customThe solvent was evaporated under a reduced pressure
5. customto give a residue, which
6. customwas then purified by silica gel column chromatography (Fuji Silysia NH, eluent; hexane:ethyl acetate=1:2 to 1:8)
7. customThe solvent was evaporated under a reduced pressure
8. customto give a residue, which
9. customwas then dried in vacuum