Potassium Carbonate → Methyl 2,4-dichloro-(2-hydroxyiminobut-3-en-4-yl)benzoate

HRID 1276136ノート

反応式

HRID 1276136 の反応式
Cl.[NH2:2][OH:3].C(=O)([O-])[O-].[K+].[K+].[Cl:10][C:11]1[C:20]([CH:21]=[CH:22][C:23](=O)[CH3:24])=[C:19]([Cl:26])[CH:18]=[CH:17][C:12]=1[C:13]([O:15][CH3:16])=[O:14]>C(O)C.O>[Cl:10][C:11]1[C:20]([CH:21]=[CH:22][C:23](=[N:2][OH:3])[CH3:24])=[C:19]([Cl:26])[CH:18]=[CH:17][C:12]=1[C:13]([O:15][CH3:16])=[O:14]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 54401157Methyl 2,4-dichloro-3-(2-oxobut-3-en-4-yl)benzoate

生成物 1

HCID 73865896Methyl 2,4-dichloro-(2-hydroxyiminobut-3-en-4-yl)benzoate

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

1.8 g (25.9 mmol) of hydroxylamine hydrochloride and 1.5 g (11.0 mmol) of potassium carbonate were added to 5.0 g (18.3 mmol) of methyl 2,4-dichloro-3-(2-oxobut-3-en-4-yl)benzoate in 160 ml of ethanol, and the reaction mixture was admixed with water until a clear solution was obtained. The mixture was heated under reflux for 3 hours and then cooled and the reaction mixture was taken up in 400 ml of water and extracted with ethyl acetate. The combined organic phases were dried and the solvent was removed. Methyl 2,4-dichloro-(2-hydroxyiminobut-3-en-4-yl)benzoate was obtained in quantitative yield.

後処理

  1. customwas obtained
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 3 hours
  4. temperaturecooled
  5. extractionextracted with ethyl acetate
  6. customThe combined organic phases were dried
  7. customthe solvent was removed

出典と根拠

ORDレコード
ord-297ec87aa4804718b9836e080ac79357
出典データセット
uspto-grants-2000_12
特許番号
US06165944

反応ノート

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