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

HRID 1938886ノート

反応式

HRID 1938886 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-5eb4d8f891f94fcc8e13ca312f5894cf
出典データセット
uspto-grants-1997_12
特許番号
US05693859

反応ノート

読み込み中…