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

HRID 358284

반응식

HRID 358284 반응식
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

참가 물질

4

반응물 2

HCID 204498332-Toluene-sulphonyloxy-3-phenoxy-hydratropic acidHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 3342Fenoprofen수율 89%

시약·촉매·용매 1

HCID 935Nickel촉매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f3f0daef5bb3420fb5df1f9d4d60a4da
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04465855

연결된 노트

불러오는 중…