2-Toluene-sulphonyloxy-3-phenoxy-hydratropic acid → Fenoprofen

HRID 358284

反応式

HRID 358284 の反応式
C1(C)C(S(O[C:11]2[C:21]([O:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)=[CH:20][CH:19]=[CH:18][C:12]=2[CH:13]([CH3:17])[C:14]([OH:16])=[O:15])(=O)=O)=CC=CC=1.[H][H]>[Ni]>[O:22]([C:21]1[CH:11]=[C:12]([CH:18]=[CH:19][CH:20]=1)[CH:13]([CH3:17])[C:14]([OH:16])=[O:15])[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1

参加物

4

反応物 2

HCID 204498332-Toluene-sulphonyloxy-3-phenoxy-hydratropic acidHCID 178418361HCID 178418361、化合物

生成物 1

HCID 3342Fenoprofen収率 89%

試薬・触媒・溶媒 1

HCID 935Nickel触媒

実験手順

To a solution of 4.1 g. of 2-toluene-sulphonyloxy-3-phenoxy-hydratropic acid in 150 ml. of alcohol 24 g. of a W-6 nickel catalyst are added, and the mixture is hydrogenated at 25° C., under atmospheric pressure until a calculated amount of hydrogen is used up. The catalyst is filtered off, the filtrate is evaporated and the residue is taken up in water and acidified with a 10% aqueous hydrochloric acid solution. The separated oil is extracted with chloroform, the chloroform solution is dried over sodium sulphate and evaporated. 2.1 g. (89%) of 3-phenoxy-hydratropic acid are obtained. Melting point of the corresponding cyclohexylamine salt amounts to 151° C. to 153° C.

後処理

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

出典と根拠

ORDレコード
ord-f3f0daef5bb3420fb5df1f9d4d60a4da
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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