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

HRID 55974
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HRID 55974 반응식
[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]
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참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-833bc5b68906462099080f574e29eff0
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09434684B2

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