Toluene → HCID 136136829, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 1-(2,4-difluorophenyl)-2-(3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)ethanone (0.26 g, 0.82 mmol; Preparation #K.1), N,N-dimethylacetamide dimethyl acetal (0.22 g, 1.64 mmol) and toluene (5 mL) was heated at about 110° C. in an oil bath for about 45 min. The reaction mixture was cooled and then concentrated under reduced pressure. 1,4-Dioxane (5.0 mL) and hydrazine (0.055 g, 1.64 mmol) were added to the mixture and it was then heated at about 95° C. in an oil bath for about 1 h. The mixture was concentrated under reduced pressure and then acetic acid was added and the material was purified by RP-HPLC (Table 1, Method d). The appropriate fractions were concentrated under reduced pressure to give a solid which was collected by filtration and dried to give the title compound (0.008 g, 3%): LC/MS (Table 1, Method a) Rt=1.99 min; MS m/z: 355.2 (M+H)+.

Provenance & Evidence