反应详情

A solution of 38.4 g of 2,4-dichloro-1-nitrobenzene in 160 ml of 2-ethoxyethanol is heated to 100° C. A solution of 152.23 g of N-benzyl-4-aminopiperidine in 40 ml of 2-ethoxyethanol is then added slowly. The mixture is maintained at reflux for 5 hours. The solvent is evaporated off under vacuum and the residue is taken up in H2O, extracted with EtOAc, washed with water and dried over Na2SO4, and the solvent is evaporated off under vacuum. The residue is chromatographed on silica, eluting with isopropyl ether. 24.4 g of the expected product are obtained after crystallization from isopropyl ether, mp=84° C.

1. temperatureThe mixture is maintained
2. temperatureat reflux for 5 hours
3. customThe solvent is evaporated off under vacuum
4. extractionextracted with EtOAc
5. washwashed with water
6. dry with materialdried over Na2SO4
7. customthe solvent is evaporated off under vacuum
8. customThe residue is chromatographed on silica
9. washeluting with isopropyl ether