反应详情

In pre-dried apparatus, held under a CaCl2 guard tube, 2,5-dibromopyridine (0.524 g), tert-butyl piperazine-1-carboxylate (0.824 g) and sodium carbonate (0.234 g) were combined in anhydrous 1-methyl-2-pyrrolidinone (10 ml) and heated in an oil bath held at 100° C. for 4 days. The mixture was then cooled, poured onto water (350 ml) and extracted with diethyl ether (3×50 ml). The combined organic extracts were washed with 2% citric acid solution (2×25 ml), water (2×25 ml), saturated brine (20 ml), dried (Na2SO4) and evaporated under reduced pressure. The residue was then purified by silica gel column chromatography, with 30% diethyl ether/hexane as eluent, to provide the title compound as a white solid (0.537 g, 71%).

1. temperatureheated in an oil bath
2. temperatureThe mixture was then cooled
3. additionpoured onto water (350 ml)
4. extractionextracted with diethyl ether (3×50 ml)
5. washThe combined organic extracts were washed with 2% citric acid solution (2×25 ml), water (2×25 ml), saturated brine (20 ml)
6. dry with materialdried (Na2SO4)
7. customevaporated under reduced pressure
8. customThe residue was then purified by silica gel column chromatography, with 30% diethyl ether/hexane as eluent