1-正丁基杂氮硅三环的合成及表征

Synthesis and Characterization of 1-n-Butylsilatrane

以正溴丁烷和镁屑为原料,制备了正丁基溴化镁;然后与正硅酸乙酯通过格氏反应,合成出正丁基三乙氧基硅烷;再与三乙醇胺在丙酮溶剂中、在氢氧化钠催化下,通过酯交换反应合成出1-丁基杂氮硅三环。研究了溶剂种类、催化剂种类、三乙醇胺与正丁基三乙氧基硅烷的量之比、反应时间对1-正丁基杂氮硅三环产率的影响,并用IR、GC-MS等对产物结构进行了表征。结果表明,格氏反应的平均产率为83.4%;酯交换反应的适宜条件为催化剂氢氧化钠的用量为三乙醇胺质量的2%、三乙醇胺与正丁基三乙氧基硅烷的量之比为2∶1、在丙酮回流温度下反应4h时,在此条件下目标产物的平均产率为73.6%。

n-butyltriethoxysilane is prepared from tetraethoxysilane and n-butylmagnesium bromide.Then 1-n-butylsilatrane is synthesized by transesterification with n-butyltriethoxysilane and triethanolamine as raw materials,acetone as solvent,sodium hydroxide as catalyst.The effects of sorts of solvent and catalyst,mole ratio between triethanolamine and n-butyltriethoxysilane,reaction time on the yield of 1-n-butylsilatrane are investigated.Meanwhile,the products are characterized by IR and GC-MS.The result shows that the average yield of the final products can be 73.6% when the amount of the sodium hydroxide catalyst is two percents of triethanolamine,the mole ratio of triethanolamine and n-butyltriethoxysilane is 2∶1,and the reaction is taken place under the refluxing temperature of acetone for 4 hours.