反应详情

温度

70 °C

244 mg of 3-(4-bromophenyl)-6-(2,6-difluorophenyl)-[1,2,4]triazine are placed in 1.8 ml of 1,2-dimethoxyethane, and 2.5 mg of bis(triphenylphosphine)palladium(II) dichloride, 159 mg of 4-trifluoromethoxyphenylboric acid and 176 mg of sodium hydrogen carbonate in 1.8 ml of water are added in succession. The reaction mixture is then heated at 70° C. for 5 h. After cooling to room temperature, the suspension is poured into 1N sodium hydroxide solution and extracted with ethyl acetate. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated. The crude product is dissolved in a minimum of hot ethyl acetate, filtered clear and crystallised at 0° C. In this way the title compound having a melting point of 199-202° C. is obtained.

1. temperatureAfter cooling to room temperature
2. extractionextracted with ethyl acetate
3. washThe organic phase is washed with saturated sodium chloride solution
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. dissolutionThe crude product is dissolved in a minimum of hot ethyl acetate
8. filtrationfiltered clear
9. customcrystallised at 0° C
10. customis obtained