反应详情

温度

85 °C

2-methoxy-4-trifluoromethoxybenzene boronic acid (72 g, 0.31 mol), K2CO3 (80.16 g, 0.58 mol) and water (100 ml) are added to a solution of 2-chloro-3-methyl -5-nitro-pyridine (50 g, 0.29 mol) in DME (500 ml) at room temperature. Pd(Ph3P)4 (3.35 g, 2.9 mmol) is added and the mixture is stirred at 85° C. for 19 hours. 500 ml of water is added and the mixture is extracted with EtOAc. The combined extracts are washed with brine and dried over Na2SO4. After removal of the solvent under reduced pressure, the residue is purified by flash column chromatography (hexane/EtOAc 9:1) to obtain 2-(2-methoxy-4-trifluoromethoxy-phenyl)-3-methyl-5-nitro-pyridine. Rf (hexane/EtOAc=9:1)=0.41.

1. extractionthe mixture is extracted with EtOAc
2. washThe combined extracts are washed with brine
3. dry with materialdried over Na2SO4
4. customAfter removal of the solvent under reduced pressure
5. customthe residue is purified by flash column chromatography (hexane/EtOAc 9:1)