季铵盐类相转移催化剂TPBAB的合成研究及应用  

Synthesis and Application of Quaternary Ammonium Salt Phase Transfer Catalyst TPBAB

作　　者：王曼 邓云龙 尤然 Wang Man;Deng Yunlong;You Ran(Department of Chemistry and Chemical Engineering,Taiyuan Institute of Technology,Taiyuan Shanxi 030008,China)

机构地区：[1]太原工业学院化学与化工系,山西太原030008

出　　处：《山西化工》2024年第9期29-33,70,共6页Shanxi Chemical Industry

摘　　要：本课题拟采用三正丙胺与溴代正丁烷为主要原料,通过加热-回流-旋转-蒸发-冷却-结晶-干燥-抽滤-过滤等工艺,制备出三丙基丁基溴化铵(TPBAB)相转移催化剂。在实验过程中,对反应溶剂、反应温度、反应时间、物料比、结晶溶剂等条件进行了研究,并利用响应面法确定了合成TPBAB的最佳工艺条件:物料比n(三正丙胺)∶n(溴代正丁烷)=1∶1.1,反应温度80℃,反应时间12 h,反应溶剂乙腈,结晶溶剂乙酸乙酯为最佳合成工艺。用红外光谱、HNMR、HPLC等方法对其进行了定性分析。实验结果表明,所获得的产物确实含有目标物质。通过在诺氟沙星苄基衍生物合成的应用中,证明所得产物具有一定的活性。Heterogeneous reaction is an important subject in organic synthesis.The phase transfer catalyst of tripropyl butyl ammonium bromide(TPBAB)was prepared by heating-refluxing-rotating-evaporating-cooling-crystallizing-drying-suction filtration-filtration.During the experiment,the reaction solvent,reaction temperature,reaction time,material ratio,crystallization solvent and other conditions were studied,and the optimum technological conditions for synthesizing TPBAB were determined by response surface method:material ratio n(tri-n-propylamine):n(n-butyl bromide)=1:1.1,reaction temperature:80℃,reaction time:12 h,and reaction solvent:acetonitrile.It was qualitatively analyzed by IR,HNMR and HPLC.From the results,the obtained product does contain the target substance.Through the application in the synthesis of benzyl derivatives of norfloxacin,it is proved that the obtained products have certain activity.

关 键 词：季铵盐类相转移催化剂 三丙基丁基溴化铵 定性分析 产品表征 

分 类 号：TQ426[化学工程]