反应详情

温度

80 °C

5-Bromo-2-(4-cyclohexyl-3-trifluoromethyl-benzyloxy)-pyridine (332 mg, 0.8 mmol), tert-butyl 1-piperazine-carboxylate (178 mg, 0.96 mmol), Pd(dppf)Cl2 (17.5 mg, 0.024 mmol), dppf (20 mg, 0.036 mmol) and sodium tert-butoxide (115 mg, 1.19 mmol) are mixed in toluene (2 mL). The mixture is purged with N2 (g), heated at 80° C. for 14 h, poured into saturated aqueous NaHCO3 and extracted with EtOAc. The combined extracts are washed with brine and dried over Na2SO4. After concentration, the residue is purified by silica gel chromatography (180:25:1 hexanes/EtOAc/Et3N) to give 4-[6-(4-Cyclohexyl-3-trifluoromethyl-benzyloxy)-pyridin-3-yl]-piperazine-1-carboxylic acid tert-butyl ester.

1. customThe mixture is purged with N2 (g)
2. additionpoured into saturated aqueous NaHCO3
3. extractionextracted with EtOAc
4. washThe combined extracts are washed with brine
5. dry with materialdried over Na2SO4
6. concentrationAfter concentration
7. customthe residue is purified by silica gel chromatography (180:25:1 hexanes/EtOAc/Et3N)