Acetic Acid → 4-[3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)-3,4-dihydro-2H-pyrrol-5-yl]-2-(trifluoromethyl)benzoic acid

HRID 1692573ノート

反応式

HRID 1692573 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:10]2([C:27]([F:30])([F:29])[F:28])[CH2:14][C:13]([C:15]3[CH:22]=[CH:21]C(C#N)=[C:17]([C:23]([F:26])([F:25])[F:24])[CH:16]=3)=[N:12][CH2:11]2)[CH:5]=[C:6]([Cl:9])[C:7]=1[Cl:8].O.[CH3:32][C:33]([OH:35])=[O:34]>OS(O)(=O)=O.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:10]2([C:27]([F:28])([F:30])[F:29])[CH2:14][C:13]([C:15]3[CH:22]=[CH:21][C:32]([C:33]([OH:35])=[O:34])=[C:17]([C:23]([F:24])([F:25])[F:26])[CH:16]=3)=[N:12][CH2:11]2)[CH:5]=[C:6]([Cl:9])[C:7]=1[Cl:8]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 962WaterHCID 582709654-[3-(3,4,5-Trichlorophenyl)-3-(trifluoromethyl)-3,4-dihydro-2H-pyrrol-5-yl]-2-(trifluoromethyl)benzonitrile

生成物 1

HCID 582709924-[3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)-3,4-dihydro-2H-pyrrol-5-yl]-2-(trifluoromethyl)benzoic acid収率 82%

試薬・触媒・溶媒 1

HCID 21910475Sulfuric acid hydrate (1:1)溶媒

実験手順

4-[3-(3,4,5-Trichlorophenyl)-3-(trifluoromethyl)-3,4-dihydro-2H-pyrrol-5-yl]-2-(trifluoromethyl)benzonitrile (0.82 g, 1.68 mmol) was dissolved in AcOH and suspended in conc. H2SO4—H2O mixture. The reaction mixture was stirred vigorously and refluxed for 26 hours. The reaction mixture was then poured to a mixture of ice and water. The resulting mixture was then extracted with EtOAc and the organic layer was washed with brine and dried over Na2SO4. The solvent was evaporated to obtain the product (0.70 g, 82%).

後処理

  1. temperaturerefluxed for 26 hours
  2. extractionThe resulting mixture was then extracted with EtOAc
  3. washthe organic layer was washed with brine
  4. dry with materialdried over Na2SO4
  5. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-a7337517cb994651b07eec0b46c29035
出典データセット
uspto-grants-2012_04
特許番号
US08158560B2

反応ノート

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