HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl Acetate → 4,5-Dihydro-1-(4-fluorophenyl)-5-[4-(methylthio)phenyl]pyrazol-3-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | 4-Fluorophenylhydrazine hydrochloride | HCID 69981 | — |
| Edukt | 3-[4-(Methylthio)phenyl]acrylonitrile | HCID 4239680 | — |
| Edukt | Sodium | HCID 5360545 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 4,5-Dihydro-1-(4-fluorophenyl)-5-[4-(methylthio)phenyl]pyrazol-3-amine | HCID 10494529 | 67,6% |
Reaktionsschritte
4-Fluorophenylhydrazine hydrochloride 4 g) was added to a solution of sodium (1.13 g) in ethanol (50 ml), and the mixture was refluxed for 1 hour. To the cooled mixture was added 3-[4-(methylthio)phenyl]acrylonitrile (4.3 g), and the resulting mixture was refluxed overnight. Ethyl acetate and water were added, and the organic layer was separated, dried and concentrated. The oily residue (7.6 g) was purified by column chromatography on silica gel (76 g) eluting with a mixture of toluene and ethyl acetate (2:1) to give brown crystals of 4,5-dihydro-1-(4-fluorophenyl)-5-[4-(methylthio)phenyl]pyrazol-3-amine (5 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05134142 |
| Quelldatensatz | uspto-grants-1992_07 |
| ORD ID | ord-2425888f196f492396fa15bd73dac99d |
| Quellennotiz | uspto-grants-1992_07 |