Ethyl cyanoacetate → HCID 57929844, compound

Participants

Reaction Conditions

Reaction Steps

6-Chloro-3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazine (5.00 g, 25.4 mmol, Preparation #G.1) and ethyl 2-cyanoacetate (3.16 g, 28.0 mmol) were added to DMF (50 mL) then the solution was cooled to about 0° C. Sodium hydride (60% in oil, 1.22 g, 30.5 mmol) was added then the mixture was stirred for about 5 min at ambient temperature and at about 60° C. for about 14 h. The mixture was cooled to ambient temperature then concentrated under reduced pressure. The residue was stirred with EtOAc (100 mL) and 2N HCl (50 mL) for about 10 min and the insoluble material was collected by filtration and dried to give the title compound (1.16 g, 17%): LC/MS (Table 1, Method g) Rt=1.53 min; MS m/z: 273.9 (M+H)+.

Provenance & Evidence