Hydrochloric Acid → HCID 68552167, compound

Temperature

0 °C

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).

1. temperatureThe mixture is heated
2. temperatureto reflux for 3 h
3. concentrationconcentrated in vacuo
4. additionCH3CN is added to the residue
5. filtrationthe mixture is filtered
6. concentrationThe filtrate is concentrated in vacuo
7. additionCH3CN is added to the residue
8. stirringwith stirring
9. filtrationthe mixture is filtered
10. concentrationThe filtrate is concentrated in vacuo

ORD record

ord-49dc4837254c48a8aea68b2d3aefeee9

Source dataset

uspto-grants-2012_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08258130B2