羟基保护－硅氢加成合成1,3-双(γ-羟丙基)-1,1,3,3-四甲基二硅氧烷

Hydroxyl protection - hydrosilylation method to prepare 1,3-bis(γ-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane

摘要:

四乙氧基硅烷与烯丙醇在乙醇钠催化下发生酯交换反应，得到一元交换产物三乙氧基烯丙氧基硅烷（Ⅰ）。将Ⅰ与1,1,3,3-四甲基二硅氧烷在铂催化剂条件下进行硅氢加成反应得到1,3-二(γ-三乙氧硅氧基丙基)-1,1,3,3-四甲基二硅氧烷（Ⅱ），Ⅱ在氢氧化钠水溶液和乙醇以质量比1:1配成的混合溶液均相水解得到1,3-双(γ-羟丙基)-1,1,3,3-四甲基二硅氧烷。以1，1，3，3-四甲基硅氧烷计算，总得率为76.4%。采用红外光谱、核磁共振、气相色谱/质谱联用等方法对中间体及产物进行了结构表征。

Abstract:

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.