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

HRID 55972

Reaktionsgleichung

Reaktionsgleichung von HRID 55972
[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]

Komponenten

4

Edukt 2

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

Produkt 1

HCID 1180716162-bromo-1-(2,4-dichlorophenyl)ethanone-O-methyloximeAusbeute 86,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-30e9a61033b64db4abdfb2063d86c16e
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09434684B2

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