反应详情

温度

50 °C

2-Benzyl-4-Chloro-5-(4-chloro-phenyl)-2H-pyridazin-3-one (3.19 g, 9.65 mmol) was dissolved in toluene (50 mL). Aluminum chloride (AlCl3, 3.22 g, 24.1 mmol) was then added and the reaction mixture was heated at 50° C. After 20 min, the reaction mixture was cooled to RT and then poured into ice-water (200 mL). The resultant solution was extracted with EtOAc (3×200 mL). The combined organic layers were washed with water (500 mL). The organic layer was dried (MgSO4), filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using EtOAc to give the title compound, 4-chloro-5-(4-chlorophenyl)-2H-pyridazin-3-one (2.33 g) as a white solid. HPLC: 2.74 min.

1. temperaturethe reaction mixture was cooled to RT
2. extractionThe resultant solution was extracted with EtOAc (3×200 mL)
3. washThe combined organic layers were washed with water (500 mL)
4. dry with materialThe organic layer was dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by column chromatography on silica gel