Reaktion #1491644

ord-b3137b504a674708812e16f85ba7d034

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    WaschenThe organic solution is subsequently washed with 1 M KHSO4, 5% NaHCO3 and brine
  2. 2
    TrocknenAfter drying over Na2SO4, dichloromethane
  3. 3
    Sonstigeis removed in vacuo
  4. 4
    Sonstigethe crude material is purified by flash chromatography (silicagel, ethyl acetate/toluene 1:4)
  5. 5
    workup.ADDITIONThe fractions containing 1-(2-phenylmorpholin-4-yl)pentan-1-one
  6. 6
    Sonstigeare collected
  7. 7
    Sonstigethe solvent is removed in vacuo

Vorschrift

A solution of 2-phenylmorpholine (326 mg, 2 mmol) in dry dichloromethane (6 mL) is cooled in an ice bath, and pentanoyl chloride (301 mg, 2.5 mmol, 1.25 eq) and triethylamine (417 μL, 3 mmol, 1.5 eq) are added. After stirring for 6 hours at room temperature the reaction mixture is diluted with dichloromethane (10 mL). The organic solution is subsequently washed with 1 M KHSO4, 5% NaHCO3 and brine. After drying over Na2SO4, dichloromethane is removed in vacuo and the crude material is purified by flash chromatography (silicagel, ethyl acetate/toluene 1:4). The fractions containing 1-(2-phenylmorpholin-4-yl)pentan-1-one are collected and the solvent is removed in vacuo to give 412 mg of colorless oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08912329B2uspto-grants-2014_12