HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 178469261, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 1,3-Diethyl 2-acetylpropanedioate | HCID 136365 | — |
| Reactant | HCID 178424562 | HCID 178424562 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 178469261 | HCID 178469261 | 36.6% |
Reaction Steps
Acetic acid (5 mL) was added to a solution of 4-mesityl-3-methyl-1H-5-pyrazoleamine (5 g, 23.22 mmol) and diethyl 2-acetylmalonate (4.7 g, 23.22 mmol) in xylene (40 mL), followed by heating under reflux for seven hours. The reaction mixture was evaporated as it was, and water was added thereto. After extracting with ethyl acetate, the organic layer was washed with an aqueous saturated sodium bicarbonate and brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (20% ethyl acetate/hexane), to give the title compound (3 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06927221B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-2eee9db2ba4e47358d3fca9c5d4a818f |
| Source note | uspto-grants-2005_08 |