Tetraethoxysilane was reacted with allyl alcohol under the condition of sodium catalyst in ethanol, and the main product was triethoxyallyloxylsilane(I). I was reacted with 1,1,3,3-tetramethyldisiloxane in the presence of Platinum compound, and obtained 1,3-(γ-3-ethoxysiliconoxy-propyl)-1,1,3,3–tetramethyldisiloxane（II）.1,3-bis(γ-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane was received by homogeneous hydrolysiss of II in the mixed solvent of 2%Sodium hydroxide solution and ethanol. With the total yield of 76.4% in terms of 1,1,3,3-tetramethyldisiloxane. IR, HNMR, Gas chromatography / Mass spectrometry were used to characterize the intimidates and target product.