反应详情

温度

0 °C

To a solution of (4-cyclohexyl-3-trifluoromethyl-phenyl)-methanol (258 mg, 1.0 mmol) in DMF (7 mL) is added sodium hydride (60% in mineral oil, 60 mg, 1.5 mmol) at 0° C. and the reaction mixture is stirred at 0° C. for 30 minutes. After the addition of a solution of 2-chloro-5-bromopyridine (231 mg, 1.2 mmol) in DMF (3 mL), the reaction mixture is stirred at 0° C. for 1 h and at room temperature for 18 hours. The reaction mixture is poured into saturated aqueous NH4Cl 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 (19:1 hexanes/EtOAc) to give 5-Bromo-2-(4-cyclohexyl-3-trifluoromethyl-benzyloxy)-pyridine.

1. stirringthe reaction mixture is stirred at 0° C. for 1 h and at room temperature for 18 hours
2. extractionextracted with EtOAc
3. washThe combined extracts are washed with brine
4. dry with materialdried over Na2SO4
5. concentrationAfter concentration
6. customthe residue is purified by silica gel chromatography (19:1 hexanes/EtOAc)