Potassium Hydroxide → Fenoprofen

HRID 2058550

Reaktionsgleichung

Reaktionsgleichung von HRID 2058550
[K+].[K+].S([O-])([O-])(=O)=O.O[C:9]1[C:19]([O:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[CH:18][CH:17]=[CH:16][C:10]=1[CH:11]([CH3:15])[C:12]([OH:14])=[O:13].[OH-].[K+]>[Ni].O>[O:20]([C:19]1[CH:9]=[C:10]([CH:16]=[CH:17][CH:18]=1)[CH:11]([CH3:15])[C:12]([OH:14])=[O:13])[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

Komponenten

5

Edukt 2

HCID 14797Potassium HydroxideHCID 705149352-Hydroxy-3-phenoxy-hydratropic acid sulphate dipotassium salt

Produkt 1

HCID 3342FenoprofenAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To a solution of 4.2 g. of 2-hydroxy-3-phenoxy-hydratropic acid sulphate dipotassium salt in 50 ml. of water 2 g. of potassium hydroxide and 2 g. of a Raney nickel catalyst prepared freshly according to Urushibara, and the reaction mixture is stirred at 60° C. for 10 to 15 minutes. The catalyst is filtered off and the filtrate is acidified with a 20% aqueous hydrochloric acid solution. The separated solution is extracted with chloroform and the chloroform solution is dried over sodium sulphate and evaporated. 2.35 g. (97%) of 3-phenoxy-hydratropic acid are obtained. Melting point of the corresponding cyclohexylamine salt: 151° C. to 153° C.

Aufarbeitung

  1. filtrationThe catalyst is filtered off
  2. extractionThe separated solution is extracted with chloroform
  3. dry with materialthe chloroform solution is dried over sodium sulphate
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-5a93305dba984b35a64029bfa5da7fa6
Quelldatensatz
uspto-grants-1982_03
Patentnummer
US04317920

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