Hydrochloric Acid → HCID 54230354, Verbindung

HRID 437812Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 437812
[OH:1]O.[F:3][C:4]1[CH:25]=[CH:24][C:7]([O:8][C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:10]=2[CH2:18][C:19](=[O:23])C(O)=O)=[CH:6][CH:5]=1.Cl>[OH-].[Na+]>[F:3][C:4]1[CH:5]=[CH:6][C:7]([O:8][C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:10]=2[CH2:18][C:19]([OH:23])=[O:1])=[CH:24][CH:25]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 214270062-(4-Fluorophenoxy)-5-nitro-α-oxobenzenepropanoic acid

Produkt 1

HCID 54230354HCID 54230354, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 14798Sodium HydroxideLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

560 Ml. of a 10% aqueous solution of hydrogen peroxide are added dropwise at 0° over a period of 75 minutes to a solution of 142 g. of 2 -(4-fluoro-phenoxy)-5-nitro-phenylpyruvic acid in 2.23 liters of 10% sodium hydroxide solution cooled to 0° C. The mixture is subsequently stirred for 3 hours at 25° C. and then acidified with 500 ml. of concentrated hydrochloric acid with cooling. This mixture is extracted twice with methylene chloride. The methylene chloride solutions are washed with water, dried over sodium sulfate and concentrated in vacuo. The residue is crystallized from benzene/hexane, and there is obtained 2-(4-fluoro-phenoxy)-5-nitro-phenylacetic acid having a melting point of 129°-130° C.

Aufarbeitung

  1. extractionThis mixture is extracted twice with methylene chloride
  2. washThe methylene chloride solutions are washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue is crystallized from benzene/hexane

Quellen und Nachweise

ORD-Eintrag
ord-d1ffb0d0c27c4c8d98b312e150992ccc
Quelldatensatz
uspto-grants-1977_06
Patentnummer
US04032525

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