邻、间和对位苯甲基官能化甲基二乙氧基硅烷的合成

Synthesis of o-,m-,and p-tolylmethyldiethoxysilane

以甲基三乙氧基硅烷、金属Na、邻氯甲苯、间氯甲苯或对氯甲苯为原料,通过伍尔兹反应合成邻、间和对位苯甲基官能化的甲基二乙氧基硅烷,利用傅里叶红外光谱(FT-IR)、核磁共振仪(NMR)、气相色谱-质谱联用仪(GC-MS)等手段对产物结构进行表征。通过正交试验方法考察反应温度、原料滴加时间、原料物质的量之比等因素对目标产物产率的影响,利用方差分析确定各个反应的最佳反应条件。结果表明:温度对3种产物的产率影响都是显著的,而原料滴加时间和物质的量之比对3种产物产率影响均不显著,利用密度-折射率联用仪测定得到25℃时3种产物的密度分别为0.962 43、0.950 55和0.948 87 g/cm3,折射率分别为1.476 18、1.469 88和1.470 69。

The o-, m- and p-tolylmethyldiethoxysilane were prepared from the Wurtz reaction of methyltrie- thoxysilane,sodium and o-ehlorotoluene or m-chlorotoluene or p-ehlorotoluene,and characterized by Fou- rier transform infrared spectrometry（ FF-IR）, gas chromatography-mass spectrometry（GC-MS） and nuclear magnetic resonance （NMR）. The orthogonal design method was used to investigate the influences of the molar ratio among the feed stocks, the reaction temperature and the feeding time on the yield of the final product. The optimum conditions in the preparation of each chemical were determined through the vari- ance analysis. The results indicated that the yields of these three compounds were significantly influenced by the reaction temperature while insignificantly affected by the feeding time and the molar ratio between the feed stocks. The densities and the refractive indexes of these three compounds were simultaneously measured by the density-refraction index analyzer at 25 ℃. Results were 0. 962 43,0. 950 55, and 0. 948 87 g/cm3 for densities,and 1. 476 18,1. 469 88, and 1. 470 69 for refractive index,respectively.