相转移催化剂TEBAB的合成研究及催化活性测试

The synthesis research of three ethyl butyl ammonium bromide(TEBAB)and catalytic activity test

相转移催化剂可改善反应条件,提高收率,使反应慢、产率低的非均相反应正常进行.但是合成成本高,很难实现工业化生产.根据季铵盐类相转移催化剂的烷基化合成原理,设计并合成出未见文献报道的新型季铵盐类相转移催化剂三乙基丁基溴化铵（TEBAB）,以降低成本,提高市场竞争力.该合成以三乙胺和溴代正丁烷为原料,DMF为反应溶剂进行反应,考查了配料比、反应温度、反应时间等条件对产物产率的影响,应用三因素三水平的正交实验法确定该合成的最佳工艺条件为：配料比为1.0∶1.5,反应温度102℃,反应时间1h.经过熔点测定和傅立叶变换红外光谱仪对其进行结构表征确认,产品的熔点为99.6℃～102.4℃,红外谱图分析确认所合成产品为目的物.最后,通过诺氟沙星衍生物合成的相转移催化反应实验验证了其催化活性.

Phase transfer catalyst can improve the reaction conditions to improve the yield, which makes the heterogeneous reac- tion with slow reaction rate and low yield product normally. But the cost of synthesis is high, it is difficult to achieve industrial production. According to the principles of quaternary ammonium phase transfer alkylation catalyst, the novel and unreported quaternary ammonium phase transfer catalyst three ethyl butyl ammonium bromide （TEBAB） is designed and synthesized in or- der to reduce costs and improve market competitiveness. Taking the synthesis of triethylamine and bromobutane as raw materi- al, DMF as the reaction solvent reaction, this paper examines the effects of ingredients, reaction temperature, reaction time and other conditions on the yield. The application of three factors and orthogonal test of three levels determine the optimum conditions for the synthesis： the ratio of ingredients 1.0 ： 1.5, reaction temperature 102 ℃, reaction time lb. Its structural characterization is confirmed through melting point and Fourier transform infrared spectrometer. Mp is： 99.6 ℃ ~ 102.4℃. Infrared spectrum analysis confirmes that the synthesized product is synthesized. Finally, the norfloxacin derivative synthesized by phase transfer catalyzed reaction experiment shows the catalytic activity.