Three mixed diorganotin dichloride have been synthesized by the reaction of tetraorganotin RSnPh3(R=Me3SiCH2、EtMe2SiCH2、Bu)with concentrated hydrochloric acid.Their structure were characterized by 1H NMR,IR,MS.The effects of the temperature,the mole ratio of tetraorganotin to concentrated hydrochloric acid and reaction time were investigated.The experimental results showed that the method has the advantages of simple operation,quick reaction,little pollution,high yield compared with other methods;the yield was over 70% when the mole ratio of tetraorganotin to concentrated hydrochloric acid was at 1:8 under refluxing condition for 7min.