Formaldehyde → HCID 22614842, compound

Participants

Reaction Steps

A mixture of 6,7-dichloro-2,3-dimethoxy-5-[3-(3-pyridyl)-4H-1,2,4-triazol-4-yl]quinoxaline (Preparation 98, 101 mg, 0.25 mmol), paraformaldehyde (15 mg, 0.5 mmol) and dimethylamine hydrochloride (22 mg, 0.27 mmol) in acetic acid (5 mL) was heated under reflux for 5 hours. After being cooled, the mixture was concentrated under reduced pressure, water (20 mL) was added, the solution basified with aqueous potassium carbonate solution and extracted with ethyl acetate (3×20 mL). The combined organic extracts were dried (MgSO4) and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel, by gradient elution using dichloromethane:methanol (1:0 changing to 95:5, by volume) to afford the title compound (75 mg, 65%) as a white solid, mp 192-194° C.

Provenance & Evidence