Dimethylformamide dimethyl acetal → HCID 57929968, 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 (0.10 g, 0.316 mmol; Preparation #K.1), N,N-dimethylformamide dimethyl acetal (0.070 g, 0.57 mmol) and toluene (2 mL) was heated at about 110° C. in an oil bath for about 30 min. The reaction mixture was cooled and then concentrated under reduced pressure. The residue was dissolved in EtOH (2.0 mL) and then potassium acetate (0.12 g, 1.26 mmol) and hydroxylamine hydrochloride (0.090 g, 1.26 mmol) were added. The mixture was heated at about 95° C. in an oil bath for about 30 min. 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 lyophilized to give the title compound (0.063 g, 58%): LC/MS (Table 1, Method a) Rt=2.11 min; MS m/z: 342.2 (M+H)+.

Provenance & Evidence