Ethanol → 2-Phenylthio-5-trifluoromethylbenzoic acid

HRID 435715ノート

反応式

HRID 435715 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 1042312-Phenylthio-5-trifluoromethylbenzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e8563dec03664a4b842a7d5bb98c510b
出典データセット
uspto-grants-1977_02
特許番号
US04006144

反応ノート

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