4-Fluorophenylhydrazine hydrochloride → HCID 19886090, Verbindung

HRID 654777Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 654777
[C:1]1([CH3:17])[CH:6]=[CH:5][C:4]([C:7](=O)[CH2:8][C:9](=O)[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:3][CH:2]=1.Cl.[F:19][C:20]1[CH:25]=[CH:24][C:23]([NH:26][NH2:27])=[CH:22][CH:21]=1>O1CCOCC1.C(O)C>[F:19][C:20]1[CH:25]=[CH:24][C:23]([N:26]2[C:7]([C:4]3[CH:5]=[CH:6][C:1]([CH3:17])=[CH:2][CH:3]=3)=[CH:8][C:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])=[N:27]2)=[CH:22][CH:21]=1

Komponenten

5

Edukt 2

HCID 699814-Fluorophenylhydrazine hydrochlorideHCID 595052Ethyl 2,4-dioxo-4-(p-tolyl)butanoate

Produkt 1

HCID 19886090HCID 19886090, VerbindungAusbeute 41,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of ethyl 4-(4-tolyl)-2,4-dioxobutanoate (4.7 g) and 4-fluorophenylhydrazine hydrochloride (3.6 g) in dioxane (35 ml) and ethanol (35 ml) was refluxed for 5 hours. The mixture was filtered and the filtrate was concentrated in vacuo. The oily residue (8 g) was purified.by column chromatography on silica gel (130 g) eluting with chloroform to give an oil of ethyl 1-(4-fluorophenyl)-5-(4-tolyl)pyrazole-3-carboxylate (2.7 g).

Aufarbeitung

  1. temperaturewas refluxed for 5 hours
  2. filtrationThe mixture was filtered
  3. concentrationthe filtrate was concentrated in vacuo
  4. washeluting with chloroform

Quellen und Nachweise

ORD-Eintrag
ord-e9c98eacbb4a4fa49693d26d9df75d47
Quelldatensatz
uspto-grants-1992_07
Patentnummer
US05134142

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