HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 86276800, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 2-Bromopropanedial | HCID 74945 | — |
| Reactant | HCID 178437214 | HCID 178437214 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86276800 | HCID 86276800 | — |
Reaction Steps
To a solution of 4-ethyl-1H-pyrazol-3-amine (0.50 g, 4.50 mmol) and 2-bromo-malonaldehyde (1.47 g, 9.72 mmol) in ethanol (8.0 mL) was added acetic acid (1.21 mL, 21.2 mmol). The reaction mixture was refluxed for 4 h, then stored in a freezer overnight. The mixture was warmed to rt, the resulting precipitate was removed by filtration and the filtrate concentrated. The resulting residue was portioned between ethyl acetate and 1M sodium hydroxide and the organic layer was washed with brine, dried (MgSO4), filtered, concentrated and purified by CombiFlash (0 to 50% EtOAc/Hex) to give product. LCMS-ESI+: calc'd for C8H9BrN3: 226.0 (M+H+); Found: 226.1 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08987250B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-a70ceccdcc544ecf8b173e8fb04665b7 |
| Source note | uspto-grants-2015_03 |