Methanol → N-methyl-2-(2-methylphenyl)-2-hydroxyiminoacetamide

HRID 1938886노트

반응식

HRID 1938886 반응식
[CH3:1][NH:2][C:3](=[O:13])[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH3:12])=O.CO.Cl.[NH2:17][OH:18]>O>[CH3:1][NH:2][C:3](=[O:13])[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH3:12])=[N:17][OH:18]

참가 물질

5

반응물 3

HCID 887MethanolHCID 443297Hydroxyamine hydrochlorideHCID 15239356N-methyl-2-(2-methylphenyl)-2-oxoacetamide

생성물 1

HCID 73792991N-methyl-2-(2-methylphenyl)-2-hydroxyiminoacetamide

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To N-methyl-2-(2-methylphenyl)-2-oxoacetamide (5.31 g, 0.03 mol), added were methanol (30 ml) and hydroxylamine hydrochloride (4.17 g, 0.06 ml), and the reaction mixture was heated under reflux for 5 hours. After completion of the reaction, water (150 ml) was added to the reaction mixture which was then extracted with methylene chloride. The extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to give N-methyl-2-(2-methylphenyl)-2-hydroxyiminoacetamide in E-form (4.79 g; yield, 83.1%) and Z-form (0.50 g; yield, 8.7%) as colorless crystals.

후처리

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 5 hours
  3. additionwas added to the reaction mixture which
  4. extractionwas then extracted with methylene chloride
  5. dry with materialThe extract was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

출처 및 근거

ORD 기록
ord-5eb4d8f891f94fcc8e13ca312f5894cf
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05693859

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