反应详情

温度

120 °C

A mixture of 5-bromo-3,4-difluoro-2-(2-fluorophenylamino)-benzoic acid methyl ester (1.00 equiv.), dppf (0.02 equiv.), Pd2dba3 (0.01 equiv.), and Zn(CN)2 (0.60 equiv.) in NMP is stirred at 120° C. in a sealed tube. After stirring for 20 hours, the reaction mixture is cooled to room temperature and quenched with a 4:1:4 (volume) mixture solution of saturated aqueous NH4Cl-conc NH4O-water. The mixture is extracted with EtOAc. The organic layer is washed with saturated aqueous NH4Cl/concentrated NH4OH/water, and brine. The organic layer is dried over MgSO4, filtered, and concentrated under reduced pressure to give the crude material that is purified by flash column chromatography to afford the desired product.

1. stirringAfter stirring for 20 hours
2. temperaturethe reaction mixture is cooled to room temperature
3. customquenched with a 4:1:4 (volume) mixture solution of saturated aqueous NH4Cl-conc NH4O-water
4. extractionThe mixture is extracted with EtOAc
5. washThe organic layer is washed with saturated aqueous NH4Cl/concentrated NH4OH/water, and brine
6. dry with materialThe organic layer is dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customto give the crude material that
10. customis purified by flash column chromatography