Potassium Hydroxide → Fenoprofen

HRID 851467

Reaktionsgleichung

Reaktionsgleichung von HRID 851467
[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-e754ed5732d240da8bf36d05a2c33f09
Quelldatensatz
uspto-grants-1983_05
Patentnummer
US04385004

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