反应详情

温度

50 °C

The 1-(2,4-difluorophenyl)ethanone (Apollo, 1.00 g, 6.40 mmol) and 3,6-dichloropyridazine (0.95 g, 6.4 mmol) in DME (10 mL) were treated with NaH (0.512 g, 12.8 mmol, 60% dispersion in oil) then warmed at about 50° C. in an oil bath. The mixture was stirred for about 4 h then sodium hydride (0.26 g, 6.4 mmol, 60% dispersion in oil) and 3,6-dichloropyridazine (0.48 g, 3.2 mmol) were added. The reaction was heated for about 0.5 h and then quenched with acetic acid and water. The mixture was extracted with EtOAc then purified by flash chromatography on silica with EtOAc as an eluent to give the title compound (0.98 g, 57%): LC/MS (Table 1, Method a) Rt=2.34 min; MS m/z: 269.1 (M+H)+.

1. temperatureThe reaction was heated for about 0.5 h
2. customquenched with acetic acid and water
3. extractionThe mixture was extracted with EtOAc
4. customthen purified by flash chromatography on silica with EtOAc as an eluent