Hydrochloric Acid → HCID 68552167, compound

Participants

Reaction Conditions

Reaction Steps

To a slurry of N-(2,6-dimethyl-3-oxo-2,5-dihydro-3H-1,2,4-triazin-4-yl)-acetamide (0.34 g, 1.846 mmol) in MeOH (3 mL) is added concentrated HCl (0.25 mL, 2.9 mmol). The mixture is heated to reflux for 3 h. The mixture is then chilled to 0° C., adjusted to pH 12 with 1 M aqueous NaOH (2.9 mL) and concentrated in vacuo. CH3CN is added to the residue with stirring and the mixture is filtered. The filtrate is concentrated in vacuo. CH3CN is added to the residue with stirring and the mixture is filtered. The filtrate is concentrated in vacuo to afford 4-amino-2,6-dimethyl-4,5-dihydro-2H-1,2,4-triazin-3-one (˜100%)). MS: 143 (M+H); 1H NMR (300 MHz, DMSO-d6) δ 4.6-3.6 (broad peak, 2H), 4.02 (s, 2H), 3.29 (s, 3H), 1.95 (s, 3H).

Provenance & Evidence