反应详情

温度

120 °C

A mixture of 2,3-dichloropyridine (10 g, 67.5 mmol, Aldrich), tert-butyl 1-piperazinecarboxylate (12.58 g, 67.5 mmol, Aldrich), copper powder (0.5 g, 7.8 mmol) and K2CO3 (9.33 g, 67.5 mmol) in DMF (100 mL) was stirred at 120° C. for 16 h. The reaction mixture was cooled to room temperature, concentrated in vacuo and the residue was dissolved in EtOAc (200 mL). The organic solution was washed with saturated aqueous solution of NaHCO3 (50 mL) and brine (50 mL), dried over Na2SO4, and filtered. The solvent was removed in vacuo and the residue was purified by silica gel column chromatography, eluting with 15% EtOAc/hexane, to give the title compound as an orange oil. MS (ESI, pos. ion) m/z: 298 (M+1).

1. temperatureThe reaction mixture was cooled to room temperature
2. concentrationconcentrated in vacuo
3. dissolutionthe residue was dissolved in EtOAc (200 mL)
4. washThe organic solution was washed with saturated aqueous solution of NaHCO3 (50 mL) and brine (50 mL)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customThe solvent was removed in vacuo
8. customthe residue was purified by silica gel column chromatography
9. washeluting with 15% EtOAc/hexane