A cage-like tetramethylammonium silicate octamer was selectively prepared by the hydrolysis and polycondensation of tetraethoxysilane with the aqueous tetramethylammonium hydroxide in equal molar ratio.Then,the tetramethylammonium silicate octamer was silanized by chloricmethyldimethylsilane to give the cage-like octa (chloricmethyldimethylsiloxy) silsesquioxane.The resulting compound was characterized by FTIR,1HNMR and 29SiNMR.In addition,the influences of reaction conditions on the yield of product were discussed.The results showed that the optimal experiment conditions were: reaction temperature 25 ℃,reaction time 17 hours,solvent DMF,n(chloricmethyldimethylsilane)∶n(tetramethylammonium silicate octamer)=60∶1,the yield is 72.3%.