The sonolysis of organic materials was performed in an organic solvent. The evolution rates of CO and CO_2 from oxalic acid in acetic acid are similar to those in an aqueous solution. It is well known that water is a useful solvent for sonochemical reactions because the reactions proceed in this solvent. Furthermore, this solvent changes to active species under sonolysis and those species accelerate the reaction. For example, H_2O_2 and active radicals produced during sonication from water (solvent) attack to reactants. On the other hand, almost all organic solvents are inactive under ultrasonic irradiation. In fact, small amounts of products are obtained from acetic acid. Acetic acid, however, had been reported as an active solvent. Now we try a sonochemical organic reaction, such as degradation of oxalic acid, in acetic acid. As the results, higher evolution rates of CO and CO_2, which were sonolytical products from oxalic acid, were obtained in distilled acetic acid. Although rapid reaction was observed in the early stage of the reaction, the yields decreased sharply with sonication time because of changing dissolved gas suddenly. In other words, higher amount of gaseous products expelled Ar (original atmosphere) from the solvent under sonication. We would examine to maintain the higher reaction rate during all the period of sonolysis.