Reaction #709444

ord-f122abf4997840b9ad3e8c59f23c4164

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    ExtractionThen, the product was extracted twice with 300 ml of ether
  2. 2
    Otherthe ether layer thus obtained
  3. 3
    Dryingwas dried with anhydrous magnesium sulfate
  4. 4
    Concentrationconcentrated by distillation

Procedure

After mixing 10 g (0.945 mol) of tetrafluorophthalic anhydride obtained in the above step with 60 ml of water, the mixture was stirred for 3 hours at room temperature. Then, the product was extracted twice with 300 ml of ether and the ether layer thus obtained was dried with anhydrous magnesium sulfate and concentrated by distillation to provide 9.7 g (yield 90%) of tetrafluorophthalic acid as white crystals. By recrystalizing the crystals from an aqueous 6N hydrochloric acid solution, crystals having higher purity (99.5%) were obtained.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04769493uspto-grants-1988_09