双(N,N-二乙基)氨基甲基苯基硅烷的合成研究

Study on Synthesis of Bis (diethylamino) Methylphenylsilane

以甲基苯基二氯硅烷和二乙胺为原料,低温下反应,合成了双(N,N-二乙基)氨基甲基苯基硅烷。通过正交试验方法考察了反应温度、反应介质、原料量之比以及反应时间等因素对目标产物产率的影响,利用红外光谱、核磁共振等手段对产物结构进行了表征和确认。利用方差分析确定的最佳反应条件为反应温度-15℃、溶剂为乙醚,二乙胺与甲基苯基二氯硅烷的量之比为5∶1、反应时间为6h。反应体系中加入三乙胺作为酸吸收剂、且用量为甲基苯基二氯硅烷的2倍时也可提高目标产物的产率;加入三乙胺后还可使铵盐副产物的后处理更易进行。

The bis（diethylamino）methylphenylsilane was prepared from methylphenyldichlorosilane and diethylamine under low temperatures.The orthogonal design method was used to investigate the influence of the reaction temperature,the reaction solvent,the molar ratio between feed stocks and the reaction time on the yield of the final product.The structure of the final product was characterized and confirmed by FT-IR,GC-MS and NMR spectra,respectively.The best reaction conditions resulted from the variance analysis were listed as follows：the reaction temperature was-15.0℃,ether was the solvent,the molar ratio between diethylamine and methylphenyldichlorosilane was 5∶1 and the reaction time was 5 hours.The yield of the final product could be improved when triethylamine and the acid acceptor added in an amount of two times the weight of methylphenyldichlorosilane.The addition of triethylamine was also facilitating the post treatment of by-product ammonium salt.