反应详情

温度

80 °C

A solution of 7.95 g (75 mmol) of sodium carbonate in 15 ml of water was added to a mixture of 2.6 g (15 mmol) of 5-bromo-2-methylpyrimidine (Coll. Czech. Chem. Comm. 14 (1949), 223-235), of 4 g (21 mmol) of 4-(trifluoromethyl)benzene boronic acid and of 0.52 g (0.45 mmol) of tetrakis(triphenylphosphine)palladium in a mixture of 50 ml of 1,2-dimethoxy-ethane and of 30 ml of ethanol. The mixture was stirred at 80° C. for 2 hours, afterwards, it was concentrated by distilling off the major part of the organic solvents. Subsequently, the residue was extracted with 3 portions of tert.-butyl methyl ether. The combined organic phases were washed with water and brine, dried over anhydrous sodium sulfate and finally evaporated. The residue was chromatographed on silicagel with a mixture of dichloromethane/tert.-butyl methyl ether (9/1 vol./vol.) as eluent. 3 g of the title compound were obtained as greenish solid. MS: 239.2 (M+H)+.

1. concentrationafterwards, it was concentrated
2. distillationby distilling off the major part of the organic solvents
3. extractionSubsequently, the residue was extracted with 3 portions of tert.-butyl methyl ether
4. washThe combined organic phases were washed with water and brine
5. dry with materialdried over anhydrous sodium sulfate
6. customfinally evaporated
7. customThe residue was chromatographed on silicagel with a mixture of dichloromethane/tert.-butyl methyl ether (9/1 vol./vol.) as eluent