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

HRID 68452

반응식

HRID 68452 반응식
[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]>[Cl-].[Cl-].[Cl-].[Cl-].C.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]

참가 물질

7

반응물 4

HCID 962Water2회HCID 6342AcetonitrileHCID 65185Metaperiodic acidHCID 580162084-Tert-butyl-1-ethynyl-2-nitrobenzene

생성물 1

HCID 2573264-Tert-butyl-2-nitrobenzoic acid

시약·촉매·용매 2

HCID 6093376Ruthenium trichloride hydrate촉매HCID 18353858Carban tetrachloride용매

실험 절차

4-tert-Butyl-1-ethynyl-2-nitro-benzene (1.662 g, 8.176 mmol) was dissolved in 20 mL carban 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).

후처리

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

출처 및 근거

ORD 기록
ord-3637e1a262e144daa73930b96e5801ea
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822457B2

연결된 노트

불러오는 중…