Ethanol → 2-Phenylthio-5-trifluoromethylbenzoic acid

HRID 435715노트

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HRID 435715 반응식
[C:1]1([S:7][C:8]2C=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][C:9]=2C#N)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-:20].[Na+].[CH2:22]([OH:24])[CH3:23]>O>[C:1]1([S:7][C:8]2[CH:9]=[CH:12][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:14][C:23]=2[C:22]([OH:20])=[O:24])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 14895212-(Phenylthio)-5-(trifluoromethyl)benzonitrile

생성물 1

HCID 1042312-Phenylthio-5-trifluoromethylbenzoic acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

6 g of 2-(phenylthio)-5-trifluoromethyl-benzonitrile, 40 ml of 15% aqueous sodium hydroxide solution and 12 ml of ethanol are heated under reflux for 12 hours and then cooled. After the addition of 100 ml of water, the mixture is extracted with 80 ml of benzene. The aqueous phase is cooled to 0° C and acidified with concentrated hydrochloric acid. The precipitate which separates out is extracted with methylene chloride. The organic phase is washed with water until neutral, dried over sodium sulphate, filtered and evaporated. There is obtained 2-(phenylthio)-5-trifluoromethyl-benzoic acid which melts at 140°-145° C.

후처리

  1. temperatureunder reflux for 12 hours
  2. temperaturecooled
  3. extractionthe mixture is extracted with 80 ml of benzene
  4. extractionThe precipitate which separates out is extracted with methylene chloride
  5. washThe organic phase is washed with water until neutral,
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-e8563dec03664a4b842a7d5bb98c510b
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04006144

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