Synthesis of hexafluoropropyleneoxide(HFPO) was carried out in a two-phase system of an aqueous phase and an organic phase, and was done in their surface. HFPO was obtained by the reaction of aqueous hypochlorite solution used for oxidizing agent, hexafluoropropylene(HFP), organic solvent, and phase transfer catalyst with fluorinated surfactant. The reactivity of the HFP and hypochlorite solution was improved as increment of the reaction area between aqueous and organic phases by the addition of the fluorinated surfactant. Amount of HFPO composition in the gas phase product reactants mol ratio. The synthesis method and the confirmation of the products by GC/MS will be described.