HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetoacetate → Ethyl 5-methyl-1-phenyl-1H-pyrazole-4-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Reactant | Phenylhydrazine hydrochloride | HCID 60962 | — |
| Reactant | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | Ethyl 5-methyl-1-phenyl-1H-pyrazole-4-carboxylate | HCID 96680 | 87.6% |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
A mixture of ethyl acetoacetate (1.5 g, 11.5 mmol) and dimethylformamide dimethyl acetal (1.68 mL, 12.7 mmol) was stirred at 120° C. for 2 hours. The reaction solution was cooled to room temperature, and a solution of phenyl hydrazine hydrochloride (1.67 g, 11.5 mmol) in ethanol (30 mL) was then added thereto. The obtained mixture was stirred at 80° C. for 2.5 hours. The reaction solution was cooled to room temperature, and it was then concentrated under reduced pressure. The residue was purified with a fractionation purification apparatus (Biotage, ethyl acetate:hexane=1:19-3:7), so as to obtain the title compound (2.32 g, 87%) in the form of a yellow oily product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09150563B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-ee94dc121ecc421b969e6bafb5fbde2b |
| Source note | uspto-grants-2015_10 |