反应详情

温度

50 °C

To a solution of 2-benzyl-5-chloro-4-(4-chlorophenyl)pyridazin-3(2H)-one (10.2 gm, 30.8 mmol) in toluene (154 mL) was added aluminum chloride (10.3 g, 77 mmol). The mixture was stirred at 50° C. for 1 h. After this time, the solution was cooled to RT, and the reaction mixture was poured into water (200 mL). The reaction mixture was extracted with EtOAc (3×100 mL). The combined organic layers were washed with saturated NaCl. The organic layer was dried (Na2SO4), filtered and concentrated. The resulting residue was triturated with EtOAc-hexane to give the title compound, 5-chloro-4-(4-chlorophenyl)pyridazin-3(2H)-one as an off-white solid (6.8 g, 92%). LC/MS (method A): RT=2.91 min, (M+H)+=241;

1. temperatureAfter this time, the solution was cooled to RT
2. extractionThe reaction mixture was extracted with EtOAc (3×100 mL)
3. washThe combined organic layers were washed with saturated NaCl
4. dry with materialThe organic layer was dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe resulting residue was triturated with EtOAc-hexane