Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | HCID 22614854 | HCID 22614854 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 22614881 | HCID 22614881 | 56% |
Reaction Steps
A suspension of 6,7-dichloro-2,3-dimethoxy-5-[3-(3-pyridyl)-4H-1,2,4-triazol-4-yl]quinoxaline (Preparation 98, 1.008 g, 2.5 mmol) and paraformaldehyde (0.75 g, 25 mmol) in acetic acid (14 mL) was heated at 125° C. for 3 hours in a sealed vessel. After being cooled, the mixture was concentrated under reduced pressure and 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 (0.60 g, 56%) as a white solid, mp 209-210° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06376490B1 |
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| Source dataset | uspto-grants-2002_04 |
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| ORD ID | ord-06188e9521834fbeabf522b3d2ca5542 |
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| Source note | uspto-grants-2002_04 |
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