Hydrochloric Acid → Fenoprofen

HRID 614262

反応式

HRID 614262 の反応式
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

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 962Water2 回HCID 12917672alpha-Methylthio-alpha-(m-phenoxyphenyl)propionic acid

生成物 1

HCID 3342Fenoprofen収率 100.3%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 3283Diethyl Ether溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-5a24ba96578944a09c3c51a7b64bb78f
出典データセット
uspto-grants-1979_03
特許番号
US04144248

関連ノート

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