1,2-Dichloro-1-iodoperfluoroethane(DCIPFE) and 3,4-dichloro-1-iodoperfluorobutane(DCIPFB) were obtained by thermal syntheses in oxygen free condition. Synthesis of DCIPFE was done by the reaction of iodine monochloride with chlorotrifluoroethlyene(CTFE). Two isomers of CF2ClCFClI and CFCl2CF2I were obtained with the composition of 97.06% CF2ClCFClI. DCIPFB was synthesized by radical telomerization of DCIPFE with tetrafluoroethylene(TFE). The conversion was depend on the initiator used in the reaction, but the mole ratio of the reactant to initiator did not affect the compositions of the telomers with the same reactant mole ratio. The synthesis method and the confirmation of the products by GC/MS and NMR will be described.