反应详情

温度

60 °C

A mixture of 5-bromo-2-chloro-3-methylpyrimidin-4(3H)-one (0.100 g, 0.448 mmol; prepared according to the procedure of Example 46, Step B), 4-fluorobenzenamine (0.056 ml, 0.582 mmol) and NaHCO3 (0.150 g, 1.79 mmol) in n-BuOH (3 mL) was stirred at 60° C. overnight. The reaction mixture was cooled to room temperature and then diluted with EtOAc. The EtOAc layer washed with H2O and saturated aqueous NaCl. The aqueous phase was re-extracted with EtOAc. The combined EtOAc layers were dried (Na2SO4), filtered and concentrated to yield the desired product (0.132 g, 99%) as a pale yellow solid that was used without further purification.

1. customprepared
2. temperatureThe reaction mixture was cooled to room temperature
3. washThe EtOAc layer washed with H2O and saturated aqueous NaCl
4. extractionThe aqueous phase was re-extracted with EtOAc
5. dry with materialThe combined EtOAc layers were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated