HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methylhydrazine → 1,5-Dimethyl-3-ethoxycarbonylpyrazole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methylhydrazine | HCID 6061 | — |
| Edukt | Ethyl 2,4-dioxovalerate | HCID 69208 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 1,5-Dimethyl-3-ethoxycarbonylpyrazole | HCID 138577 | — |
Reaktionsschritte
9.2 ml of methylhydrazine was added dropwise over 30 minutes to a solution of 25 g of ethyl 2,4-dioxovalerate in 36 ml of ethanol, the temperature of the mixture being kept below 40° C. by cooling in an ice bath. The resulting solution was heated at reflux for 23 hours, poured into 300 ml of ice water and the resulting mixture was extracted with ether. The extract was dried (MgSO4), filtered and stripped of solvent. The residue was chromatographed on silica gel, with a 1:1 v:v mixture of ethyl acetate and hexane as eluent. The middle fractions gave ethyl 1,5-dimethylpyrazole-3-carboxylate (39A), as a yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04853027 |
| Quelldatensatz | uspto-grants-1989_08 |
| ORD ID | ord-ce029a6a88c749e598bcbe45ea6576fe |
| Quellennotiz | uspto-grants-1989_08 |