反应详情

温度

120 °C

5-Bromo-pyridine-2-carbonitrile (8 mmol), tert-butyl 1-piperazine-carboxylate (9.6 mmol), Pd(dppf)Cl2 (0.24 mmol), dppf (0.36 mmol) and sodium tert-butoxide (11.9 mmol) are mixed in toluene (12 mL) and purged with N2. The mixture is heated in a microwave reactor at 120° C. for 15 minutes, poured into saturated Na2CO3 solution and extracted with EtOAc. The combined extracts are washed with saturated aqueous NaCl and dried over Na2SO4. After concentration, the residue is purified by silica gel chromatography (2:1 hexanes/EtOAc) to give tert-butyl 4-(6-cyano-pyridin-3-yl)-piperazine-1-carboxylate.

1. custompurged with N2
2. additionpoured into saturated Na2CO3 solution
3. extractionextracted with EtOAc
4. washThe combined extracts are washed with saturated aqueous NaCl
5. dry with materialdried over Na2SO4
6. concentrationAfter concentration
7. customthe residue is purified by silica gel chromatography (2:1 hexanes/EtOAc)