HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 9802164, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 22614877 | HCID 22614877 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 9802164 | HCID 9802164 | 71.2% |
Reaction Steps
A mixture of (±)-6,7-dichloro-2,3-dimethoxy-5-[3-methoxymethyl-5-(3-pyridyl)-4H-1,2,4-triazol-4-yl]quinoxaline (3.0 g, 6.7 mmol), 2M aqueous hydrochloric acid solution (10 mL) and 1,4-dioxane (50 mL) was heated under reflux for 9 hours, cooled, and concentrated under reduced pressure. The residue was dissolved in 1M aqueous sodium hydroxide solution and acidified to pH 4.5 with concentrated hydrochloric acid to afford a thick white precipitate. This was collected by filtration and washed with water to give (±)-6,7-dichloro-5-[3-methoxymethyl-5-(3-pyridyl)-4H-1,2,4-triazol-4-yl]-2,3(1H,4H)-quinoxalinedione (2.0 g, 68%) as an off-white solid, mp 230-232° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06376490B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-a348872105414bcf882026071273be65 |
| Source note | uspto-grants-2002_04 |