Réaction #52083

ord-6e941d7d62d446969ab06bbadee4016b

Conditions de réaction

Température
50°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    TempératureThe mixture was cooled to 10° C.
  2. 2
    workup.STIRRINGthe mixture was stirred overnight
  3. 3
    AutreThe solution was subjected to liquid-liquid separation
  4. 4
    Lavagethereafter, the organic layer was washed with 40 mL of 7.5% aqueous sodium hydrogencarbonate and 40 mL of 10% aqueous sodium chloride
  5. 5
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure

Mode opératoire

To the 2,6-di-tert-butylhydroquinone obtained in Example 10, 50 mL of hexane, 13.92 g (136.5 mmol) of acetic anhydride and 0.79 g (8.06 mmol) of sulfuric acid were added and the mixture was stirred for 2 hours at 50° C. The mixture was cooled to 10° C. and after adding 30 mL of water and 10 mL of ethyl acetate, the mixture was stirred overnight. The solution was subjected to liquid-liquid separation and the aqueous layer was discarded; thereafter, the organic layer was washed with 40 mL of 7.5% aqueous sodium hydrogencarbonate and 40 mL of 10% aqueous sodium chloride and the solvent was distilled off under reduced pressure to give 1,4-diacetoxy-2,6-di-tert-butylbenzene.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06852867B2uspto-grants-2005_02