Reaktion #84251

ord-c7e38a2a4cfe4577b970b6e0f7a09925

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter completion of the reaction
  2. 2
    Extraktionextracted with ethyl acetate (50 ml×1)
  3. 3
    Waschenthe resulting organic layer was washed with water (20 ml×1)
  4. 4
    Trocknendried over saturated aqueous sodium chloride
  5. 5
    Sonstigeanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
  6. 6
    SonstigeThe resulting residue was purified by silica gel column chromatography

Vorschrift

To 2.17 g of 2-bromo-1-(2,4-dichlorophenyl)ethanone-O-methyloxime in 20 ml of N,N-dimethylformamide, 3.03 g of potassium phthalimide and 1.61 g of potassium carbonate were added, and the mixture was stirred at room temperature for 18 hours. After completion of the reaction, the reaction mixture was mixed with 40 ml of water and extracted with ethyl acetate (50 ml×1), the resulting organic layer was 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. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 1:9 to 3:7) as the eluent to obtain 2.10 g of the desired product as pale yellow crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434684B2uspto-grants-2016_09