Acetic Acid → 3,4,5,6-Tetrafluorophthalic acid

Participants

Reaction Steps

After mixing 50 g of the above dried N-cyclohexyl-tetrafluorophthalimide with 80 ml of 85% sulfuric acid, 80 ml of acetic acid was added to the mixture and it was reacted for 5 hours at 120° to 130° C. with stirring. After the reaction was completed, acetic acid was distilled off from the reaction mixture under a reduced pressure and the product was continuously extracted with toluene for 24 hours. When the toluene layer obtained was concentrated by distillation under a reduced pressure, crude crystals of yellow tetrafluorophthalic anhydride were precipitated. The concentrate was distilled under a reduced pressure (20 mmHg) at 150° C. and the crystals thus obtained were hydolyzed by adding 100 ml of an aqueous 6N hydrochloric acid solution. The hydrolyzed product was cooled and then extracted with ether to provide white crystals of tetrafluorophthalic acid (yield 90%).

Provenance & Evidence