4-Fluorophenol → Quinoxyfen

HRID 2255428Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2255428
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([Cl:13])=[CH:9][C:10]=2[Cl:12])[N:5]=[CH:4][CH:3]=1.[F:14][C:15]1[CH:20]=[CH:19][C:18]([OH:21])=[CH:17][CH:16]=1>C(OCC)(=O)C.[OH-].[Na+]>[Cl:12][C:10]1[CH:9]=[C:8]([Cl:13])[CH:7]=[C:6]2[C:11]=1[C:2]([O:21][C:18]1[CH:19]=[CH:20][C:15]([F:14])=[CH:16][CH:17]=1)=[CH:3][CH:4]=[N:5]2

Komponenten

5

Edukt 2

HCID 97324-FluorophenolHCID 6158354,5,7-Trichloroquinoline

Produkt 1

HCID 3391107QuinoxyfenAusbeute 76,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8857Ethyl AcetateLösungsmittelHCID 14798Sodium HydroxideLösungsmittel

Reaktionsbedingungen

Temperatur
160 °C

Versuchsvorschrift

A mixture of 29.11 g of 4,5,7-trichloroquinoline and 16.84 g of 4-fluorophenol was heated to 160° C. After approximately 40 minutes, the molten solution solidified. The solid was dissolved in ethyl acetate and 2N NaOH. The organic layer was washed with base to remove excess phenol, then dried. Solvent was removed by reducing pressure, and the residue was purified by recrystallizing in heptane to produce 29.49 g of the title product. M.P. 105°-106° C.

Aufarbeitung

  1. washThe organic layer was washed with base
  2. customto remove excess phenol
  3. customdried
  4. customSolvent was removed
  5. customthe residue was purified
  6. customby recrystallizing in heptane

Quellen und Nachweise

ORD-Eintrag
ord-070086f1772e493ba15c826b7bd9e346
Quelldatensatz
uspto-grants-1993_08
Patentnummer
US05240940

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