反应详情

A solution of 0.583 ml (9 mmol) methanesulfonic acid and, at about 30° C., ether are added to a hot solution of 1.56 g (4.5 mmol) 1-(4-chloroanilino)-4-(4-pyridylmethyl)phthalazine until slight turbidity occurs. As it cools to 0° C., crystals precipitate out; these are filtered off and recrystallized again from methanol. After drying under HV (8 h, 120° C.) and equilibration for 24 h at 20° C. and in room atmosphere, title compound is obtained with a water content of 3.97%; m.p. 145-150° C.; 1H NMR (DMSO-d6) 10.50-11.70 (br), 8.82-8.88 (m, 3H), 8.33-8.39 (m, 1H), 8.18-8.29 (m, 2H), 7.98 (d, 2H), 7.58-7.70 (m, 4H), 4.94 (s, 2H), 2.32 (s, 6H); ESI-MS: (M+H)+=347.

1. customcools to 0° C.
2. customcrystals precipitate out
3. filtrationthese are filtered off
4. customrecrystallized again from methanol
5. customAfter drying under HV (8 h, 120° C.) and equilibration for 24 h at 20° C. and in room atmosphere