Oxygen → Ketoprofen

HRID 1650020

反応式

HRID 1650020 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 3825Ketoprofen

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 14048876Cobaltous 2-naphthenic acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1c1e585117c94c9da57bc4eb0ef9a7ef
出典データセット
uspto-grants-1990_05
特許番号
US04922052

関連ノート

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