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, 100° C.), title compound is obtained with a methanol content of 1.27%; m.p. >270° C.; 1H NMR (DMSO-d6) 9.91 (s, 1H), 9.13 (s, 1H), 8.59-8.64 (m, 1H), 8.48 (d, 2H), 8.08-8.13 (m, 1H), 7.91-8.01 (m, 2H), 7.85 (d, 2H), 7.58 (d, 2H), 7.32 (d, 2H), 4.58 (s, 2H), 2,05 (s, 3H), [methanol: 4.13 (q, 0.15H), 3.19 (d, 0.45H)]; ESI-MS: (M+H)+=370.

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, 100° C.)