Reacción #1925214

ord-9a2cef41679a44e58179eb31c54cfe65

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroto terminate
  2. 2
    Otrothe reaction
  3. 3
    ExtracciónThe reaction mixture was extracted with ethyl acetate
  4. 4
    LavadoThe organic layer was then washed with water
  5. 5
    Secadodried over anhydrous sodium sulfate
  6. 6
    ConcentraciónAfter concentration under reduced pressure
  7. 7
    workup.DISTILLATIONthe residue was purified by distillation under reduced pressure

Procedimiento

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%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06673511B1uspto-grants-2004_01