反应详情

To a suspension of 3-fluoro-4-iodopyridine (2.23 g), 1-(tert-butoxycarbonyl)-4-(piperidin-4-ylcarbonyl) piperazine (1.49 g) and sodium t-butoxide (1.06 g) in 1,4-dioxan (20 ml) was added tris(dibenzylidene acetone)dipalladium(0) (0.09 g) and tri-o-tolylphosphine (0.12 g) and the mixture heated at reflux for 3 hours. The mixture was diluted with diethyl ether and washed with saturated aqueous sodium chloride solution. dried (Na2SO4) and evaporated. The residue was purified by chromatography on alumina (N32-63) eluting with 0.4% methanol in dichloromethane to give as a solid, 1-(tert-butoxycarbonyl)-4-[1-(3-fluoro-4-pyridyl)piperidin-4-ylcarbonyl]piperazine (0.70 g).

1. temperaturethe mixture heated
2. temperatureat reflux for 3 hours
3. washwashed with saturated aqueous sodium chloride solution
4. dry with materialdried (Na2SO4)
5. customevaporated
6. customThe residue was purified by chromatography on alumina (N32-63)
7. washeluting with 0.4% methanol in dichloromethane