Reacción #217449

ord-dd2ffcd1a88f49b38c951d7c4ce09a70

Disolventes

Condiciones de reacción

Temperatura
120°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroInto a 4 liter beaker equipped with magnetic stirrer
  2. 2
    TemperaturaThe mixture was then cooled to 50° C.
  3. 3
    OtroA thick white precipitate formed
  4. 4
    Filtraciónwhich was filtered
  5. 5
    Lavadowashed with 3×1 liter portions of methanol and oven
  6. 6
    Otrodried at 60° C.

Procedimiento

Into a 4 liter beaker equipped with magnetic stirrer, dropping funnel, and thermometer, was charged stearyl alcohol (270.0 grams, 1.0 mol; obtained from Sigma-Aldrich), isatoic anhydride (244.0 grams, 1.5 mol), 1,4-diazabicyclo(2.2.2)octane (DABCO) (56 grams, 0.5 mol), and dimethylformamide (750 milliliters). The mixture was stirred and heated to 120° C. for a period of about 2 hours. The mixture was then cooled to 50° C., and methanol (3 liters) was added. A thick white precipitate formed, which was filtered and then washed with 3×1 liter portions of methanol and oven dried at 60° C. to yield 295.8 grams of a beige solid at 76 percent yield.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07381253B2uspto-grants-2008_06