反应详情

4-(5-Bromopyrimidin-2-yl)piperazine-1-carboxylic acid tert-butyl ester (1.01 g), 4-fluorophenylboronic acid (0.45 g), tetrakis(triphenylphosphine)palladium(0) (0.12 g) and potassium phosphate (1.25 g) were dissolved in a mixture of 1,2-dimethoxyethane (40 ml) and water (10 ml), degassed and heated to reflux under nitrogen. After 16 h. the reaction was cooled, reduced in vacuo, dissolved in diethyl ether (100 ml) and washed with water (3×20 ml), saturated brine (20 ml), dried (Na2SO4) and evaporated. The black residue was then chromatographed on silica, with 2% methanol/dichloromethane to provide the title compound as a pale yellow solid (1.01 g, 96%).

1. customdegassed
2. temperatureheated
3. temperatureto reflux under nitrogen
4. temperatureAfter 16 h. the reaction was cooled
5. dissolutiondissolved in diethyl ether (100 ml)
6. washwashed with water (3×20 ml), saturated brine (20 ml)
7. dry with materialdried (Na2SO4)
8. customevaporated
9. customThe black residue was then chromatographed on silica, with 2% methanol/dichloromethane