Reacción #1069769

ord-f811ec377c934eb9b5c669d0d761692b

Reactivos

Ninguno

Condiciones de reacción

Temperatura
140°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrowhile collecting the methanol condensate
  2. 2
    TemperaturaThe reaction mixture was subsequently heated in a 200° C. at reduced pressure (1.5 mm)
  3. 3
    workup.DISTILLATIONto distill off excess diethanolamine
  4. 4
    workup.DISSOLUTIONThe highly viscous oily residue was dissolved in an equal volume of acetone
  5. 5
    OtroThe resulting crystalline solid was collected
  6. 6
    Lavadowashed with acetone
  7. 7
    Otrodried

Procedimiento

A mixture of 57.58 g (0.25 mol) dimethyl sebacate and 157.71 g (1.50 mol) of diethanolamine was heated in a 140° C. bath under nitrogen for 2.5 hrs while collecting the methanol condensate. The reaction mixture was subsequently heated in a 200° C. at reduced pressure (1.5 mm) to distill off excess diethanolamine. The highly viscous oily residue was dissolved in an equal volume of acetone and stirred overnight. The resulting crystalline solid was collected, washed with acetone, and dried. The yield of product was 35.0 g (9.3% of theory); mp=87-98° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06861192B2uspto-grants-2005_03