Hydrochloric Acid → Fenoprofen

HRID 614262

반응식

HRID 614262 반응식
O.Cl.CS[C:5]([C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:11]=1)([CH3:9])[C:6]([OH:8])=[O:7]>[Zn].C(OCC)C>[O:16]([C:12]1[CH:11]=[C:10]([CH:5]([CH3:9])[C:6]([OH:8])=[O:7])[CH:15]=[CH:14][CH:13]=1)[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 962Water2회HCID 12917672alpha-Methylthio-alpha-(m-phenoxyphenyl)propionic acid

생성물 1

HCID 3342Fenoprofen수율 100.3%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 3283Diethyl Ether용매

실험 절차

Water (1.5 ml) and 1.5 ml of conc. hydrochloric acid were added to 432 mg of α-methylthio-α-(m-phenoxyphenyl)propionic acid, and then 300 mg of zinc powder was added. With stirring, the mixture was heated under reflux for 2.5 hours. Water (10 ml) and 30 ml of diethyl ether were added to the reaction mixture. The insoluble matter was separated by filtration. The filtrate was extracted three times with 80 ml of diethyl ether. The organic layer was washed with 10 ml of water, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure to afford 364 mg of α-(m-phenoxyphenyl)propionic acid as an oil. The yield was 100%.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2.5 hours
  3. customThe insoluble matter was separated by filtration
  4. extractionThe filtrate was extracted three times with 80 ml of diethyl ether
  5. washThe organic layer was washed with 10 ml of water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-5a24ba96578944a09c3c51a7b64bb78f
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04144248

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