Reaktion #1925214

ord-9a2cef41679a44e58179eb31c54cfe65

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto terminate
  2. 2
    Sonstigethe reaction
  3. 3
    ExtraktionThe reaction mixture was extracted with ethyl acetate
  4. 4
    WaschenThe organic layer was then washed with water
  5. 5
    Trocknendried over anhydrous sodium sulfate
  6. 6
    EinengenAfter concentration under reduced pressure
  7. 7
    workup.DISTILLATIONthe residue was purified by distillation under reduced pressure

Vorschrift

At 20 to 30° C., acetic anhydride was added to a mixture of 9.29 g of N,N-bis(2-hydroxyethyl)-2-(methoxycarbonyl)ethylamine, 12.8 g of triethylamine, 50 mg of 4-dimethylaminopyridine and 50 ml of THF and the resulting mixture was stirred for 20 hours. Water was added to terminate the reaction. The reaction mixture was extracted with ethyl acetate. The organic layer was then washed with water and dried over anhydrous sodium sulfate. After concentration under reduced pressure, the residue was purified by distillation under reduced pressure, whereby 13.2 g of N,N-bis(2-acetoxyethyl)-2-(methoxycarbonyl)ethylamine was obtained (boiling point: 118 to 123° C./21 Pa, yield: 99%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06673511B1uspto-grants-2004_01