Water → HCID 9886575, compound

Participants

Reaction Steps

Sodium hydride (60% dispersion in oil, 23 mg, 0.58 mmol) was added to a solution of (2-methyl-2H-1,2,4-triazol-3-yl)methanol (EP-A-421210) (57 mg, 0.53 mmol) in dry DMF (2 ml) at room temperature under nitrogen. After 1 hour at room temperature a solution of 6-chloro-7-(3,6-dihydro-2H-pyridin-1-yl)-3-phenyl-1,2,4-triazolo[4,3-b]pyridazine (150 mg) in dry DMF (2 ml) was added via syringe. The mixture was stirred at room temperature for 16 hours. Water (20 ml) was added and the solid filtered and dried in vacuo. Recrystallisation from ethyl acetate/petroleum ether afforded the title pyridaziite as a white solid (131 mg, 70%). 1H NMR (250 MHz, CDCl3) 8.29 (2H, m), 7.94 (1H, s), 7.52 (3H, m), 7.23 (1H, s), 5.91 (1H, m), 5.80 (1H, m), 5.63 (2H, s), 3.96 (3H, s), 3.71 (2H, m), 3.40 (2H, m), 2.23 (2H, m). MS (ES+) 389 [MH]+.

Provenance & Evidence