Oxygen → Ketoprofen

HRID 1650020

반응식

HRID 1650020 반응식
[CH2:1]([C:8]1[CH:9]=[C:10]([CH:14]([CH3:18])[C:15]([OH:17])=[O:16])[CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[O:19]=O>C1C=C2C(C=C(C([O-])=O)C=C2)=CC=1.C1C=C2C(C=C(C([O-])=O)C=C2)=CC=1.[Co+2].C(O)(=O)C>[C:1]([C:8]1[CH:9]=[C:10]([CH:14]([CH3:18])[C:15]([OH:17])=[O:16])[CH:11]=[CH:12][CH:13]=1)(=[O:19])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 977OxygenHCID 109516832-(3-Benzylphenyl)propanoic acid

생성물 1

HCID 3825Ketoprofen

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 14048876Cobaltous 2-naphthenic acid용매

실험 절차

To a 300 ml reaction vessel with a stirrer were fed 25 g of α-(3-benzylphenyl)propionic acid obtained in Experiment 5, 0.08 g of cobalt naphthenate and 100 ml of acetic acid as a solvent, and 150 ml/min of pure oxygen was fed into the vessel for 16 hours at a reaction temperature of 120 ° C. After the reaction, the solvent was removed by reduced-pressure distillation to obtain a solid substance. The solid substance was washed five times with 500 ml of water and it was dissolved in 500 ml of ether and washed three times again with water. After that, the ether was removed by reduced-pressure distillation and the product was finally recrystallized with a benzene/petroleum ether mixture to obtain 13.2 g of α-(3-benzoylphenyl)propionic acid (ketoprofen). The properties such as melting point and spectrum of the final product were the same as those of an authentic sample.

후처리

  1. customTo a 300 ml reaction vessel with a stirrer
  2. customAfter the reaction
  3. customthe solvent was removed by reduced-pressure distillation
  4. customto obtain a solid substance
  5. washThe solid substance was washed five times with 500 ml of water and it
  6. dissolutionwas dissolved in 500 ml of ether
  7. washwashed three times again with water
  8. customAfter that, the ether was removed by reduced-pressure distillation
  9. customthe product was finally recrystallized with a benzene/petroleum ether mixture

출처 및 근거

ORD 기록
ord-1c1e585117c94c9da57bc4eb0ef9a7ef
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04922052

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