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2-Bromo-1-(2,4-dichlorophenyl)ethan-1-one → 2-bromo-1-(2,4-dichlorophenyl)ethanone-O-methyloxime

HRID 55972
ノート
印刷プレビュー

反応式

HRID 55972 の反応式
[Br:1][CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:6]=1[Cl:12])=O.Cl.[CH3:14][O:15][NH2:16]>C(O)C>[CH3:14][O:15][N:16]=[C:3]([C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:6]=1[Cl:12])[CH2:2][Br:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 758282-Bromo-1-(2,4-dichlorophenyl)ethan-1-oneHCID 521874O-Methylhydroxylamine hydrochloride

生成物 1

HCID 1180716162-bromo-1-(2,4-dichlorophenyl)ethanone-O-methyloxime収率 86.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To 4.00 g of 2-bromo-1-(2,4-dichlorophenyl)ethanone in 20 ml of ethanol, 1.25 g of methoxyamine hydrochloride was added, and the mixture was stirred at room temperature for 12 hours. After completion of the reaction, the solvent was evaporated under reduced pressure, and the resulting residue was mixed with 20 ml of water and extracted with ethyl acetate (20 ml×2). The resulting organic layers were combined, washed with water (20 ml×1) and then dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain 3.85 g of the desired crude product as a pale yellow oil. The oil was used in the next step without further purification.

後処理

  1. customAfter completion of the reaction
  2. customthe solvent was evaporated under reduced pressure
  3. additionthe resulting residue was mixed with 20 ml of water
  4. extractionextracted with ethyl acetate (20 ml×2)
  5. washwashed with water (20 ml×1)
  6. dry with materialdried over saturated aqueous sodium chloride
  7. customanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-30e9a61033b64db4abdfb2063d86c16e
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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