反应详情

温度

110 °C

A mixture of 0.511 g (2 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine, 0.901 g (6 mmol) 4-aminoacetanilide and 5 ml 1-butanol is heated for 3 h at 110° C. The reaction mixture is then evaporated under vacuum, the crystalline residue is taken up in a mixture of 20 ml dichloromethane and 10 ml 20% aqueous potassium carbonate solution while stirring, then filtered and the filter residue washed with water and dichloromethane. After recrystallization from dichloromethane/methanol and drying under HV (8 h, 1 00° C.), title compound is obtained with a methanol content of 1.27%;

1. customThe reaction mixture is then evaporated under vacuum
2. additionthe crystalline residue is taken up in a mixture of 20 ml dichloromethane and 10 ml 20% aqueous potassium carbonate solution
3. filtrationfiltered
4. washthe filter residue washed with water and dichloromethane
5. customAfter recrystallization from dichloromethane/methanol
6. customdrying under HV (8 h, 1 00° C.)