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Water → 2-amino-1-(2,4-dichlorophenyl)ethanone-O-methyloxime

HRID 55974
ノート
印刷プレビュー

反応式

HRID 55974 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9](=[N:22][O:23][CH3:24])[CH2:10][N:11]1C(=O)C2=CC=CC=C2C1=O.O.NN.O>C(O)C>[CH3:24][O:23][N:22]=[C:9]([C:3]1[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=1[Cl:1])[CH2:10][NH2:11]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 118071602N-[2-(2,4-dichlorophenyl)-2-(methoxyimino)ethyl]phthalimide

生成物 1

HCID 1180715922-amino-1-(2,4-dichlorophenyl)ethanone-O-methyloxime収率 83.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

To 316 mg of N-[2-(2,4-dichlorophenyl)-2-(methoxyimino)ethyl]phthalimide in 10 ml of ethanol, 108 mg of hydrazine monohydrate was added, and the mixture was stirred at 60° C. for 2 hours. After completion of the reaction, the reaction mixture was allowed to cool to room temperature, mixed with 30 ml of water and extracted with ethyl acetate (40 ml×1). The resulting organic layer was dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain 170 mg of the desired crude product as a colorless oil. The oil was used in the next step without further purification.

後処理

  1. customAfter completion of the reaction
  2. temperatureto cool to room temperature
  3. extractionextracted with ethyl acetate (40 ml×1)
  4. dry with materialThe resulting organic layer was dried over saturated aqueous sodium chloride
  5. customanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-833bc5b68906462099080f574e29eff0
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434684B2

反応ノート

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