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

HRID 55972
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HRID 55972 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-30e9a61033b64db4abdfb2063d86c16e
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09434684B2

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