Potassium Hydroxide → Fenoprofen

HRID 358285

反応式

HRID 358285 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 Urashibara, 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-42ffd2605ef546f4b2cf9b328b128d26
出典データセット
uspto-grants-1984_08
特許番号
US04465855

関連ノート

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