Potassium Hydroxide → Fenoprofen

HRID 851467

反応式

HRID 851467 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 3342Fenoprofen収率 97%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e754ed5732d240da8bf36d05a2c33f09
出典データセット
uspto-grants-1983_05
特許番号
US04385004

関連ノート

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