Water → 4-Tert-butyl-2-nitrobenzoic acid

HRID 1644198

反応式

HRID 1644198 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]#C)=[C:7]([N+:13]([O-:15])=[O:14])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].C(#N)C.I(O)(=O)(=O)=[O:20].[OH2:24]>C(Cl)(Cl)(Cl)Cl.O.[Ru](Cl)(Cl)Cl>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]([OH:20])=[O:24])=[C:7]([N+:13]([O-:15])=[O:14])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

7

反応物 4

HCID 962Water2 回HCID 6342AcetonitrileHCID 65185Metaperiodic acidHCID 580162084-Tert-butyl-1-ethynyl-2-nitrobenzene

生成物 1

HCID 2573264-Tert-butyl-2-nitrobenzoic acid

試薬・触媒・溶媒 2

HCID 6093376Ruthenium trichloride hydrate触媒HCID 5943Carbon Tetrachloride溶媒

実験手順

4-tert-Butyl-1-ethynyl-2-nitro-benzene (1.662 g, 8.176 mmol) was dissolved in 20 mL carbon tetrachloride, 20 mL acetonitrile, and 40 mL water. Periodic acid (9.322 g, 40.89 mmol) was added followed by ruthenium(III)chloride hydrate (85 mg, 0.41 mmol). After stirring of 90 minutes, the resulting mixture was diluted with water and extracted with three portions of dichloromethane. The combined dichloromethane layers wee dried over anhydrous MgSO4, and concentrated in vacuo to yield 4-tert-Butyl-2-nitro-benzoic acid (1.924 g, 86.19 mmol).

後処理

  1. extractionextracted with three portions of dichloromethane
  2. dry with materialThe combined dichloromethane layers wee dried over anhydrous MgSO4
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-4e7e177bb8104ba1bf09655ed606f506
出典データセット
uspto-grants-2012_02
特許番号
US08124604B2

関連ノート

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