Reacción #347316

ord-dfd6bab83436493486bd1a795b68e9ad

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrofitted with an overhead stirrer
  2. 2
    TemperaturaThe mixture was heated gently
  3. 3
    Otro(61° C. to 64° C.)
  4. 4
    TemperaturaHeating
  5. 5
    Otro(147° C.)
  6. 6
    Temperaturathis temperature was maintained for a period of one hour
  7. 7
    Otroto form
  8. 8
    Filtraciónfiltered
  9. 9
    Otrorecrystallised from petroleum ether 60-80
  10. 10
    Otrowas placed in a vacuum oven at 40° C.
  11. 11
    Secadountil dry of residual acetic acid

Procedimiento

Palmitic acid (512.04 g, 2.00 moles) and acetic anhydride (204.05 g, 2.00 moles) were charged to a two liter reaction flask fitted with an overhead stirrer, thermometer, condenser and nitrogen inlet. The mixture was heated gently with stirring to allow the solid palmitic acid to melt (61° C. to 64° C.). Heating was continued until the reflux temperature had been reached (147° C.), this temperature was maintained for a period of one hour. The resultant mixture was cooled to room temperature to allow a light yellow solid to form, this was slurried in cyclohexane (100 ml), filtered and recrystallised from petroleum ether 60-80. The recrystallised wet solid was placed in a vacuum oven at 40° C. until dry of residual acetic acid. The resultant white powdery solid was stored under vacuum in the presence of silica gel. The yield of palmitic anhydride was 458.49 g which represented a 92.8% chemical yield.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05525709uspto-grants-1996_06