《药物合成反应》创新实验教学设计--电氧化4-甲基苯乙烯双硫氰基化反应  

Innovative Experimental Teaching Design in“Organic Reactions for Drug Synthesis”Course:Electrochemically Oxidative Dithiocyanidation of 4-Methylstyrene

作　　者：牟学清 杜蕾 韩文勇 崔宝东 Mou Xueqing;Du Lei;Han Wenyong;Cui Baodong(School of Pharmacy,Zunyi Medical University,Zunyi 563006,China)

机构地区：[1]遵义医科大学药学院,贵州遵义563006

出　　处：《广东化工》2024年第23期153-155,158,共4页Guangdong Chemical Industry

基　　金：贵州省高等学校教学内容和课程体系改革项目(SJJG202202177,SJJG2023179);遵义医科大学校级课程思政改革试点建设项目(XJKCSZ20213,XJKCSZ202225,XJKCSZ202315)。

摘　　要：瞄准绿色合成技术人才培养目标,本论文将电氧化4-甲基苯乙烯双硫氰基化反应的探索实验改为《药物合成反应》教学实验,丰富绿色制药人才培养体系。本实验以4-甲基苯乙烯和硫氰酸胺为原料、碳棒为阳极、铂片为阴极、四正丁基醋酸铵为电解质、电流为8毫安,在氩气条件下装有乙腈的三颈瓶中电解3.5小时,经过柱层析纯化得到目标产物,分离产率为68%。实验内容包括电解装置的搭建与调试、氩气置换、反应进程监测、柱层析分离及核磁结构表征等操作。该教学实验原料廉价易得、操作便捷、安全、用时较短,并采用线上线下混合式教学方式开展,有望发展为提升学生有机电化学理论和实验操作技能的推广性教学实验。Aiming to cultivate talents in green synthesis technologies,this work transforms the exploratory experiment of electrochemically oxidative dithiocyanidation of 4-methylstyrene into a teaching experiment of“Organic Reactions for Drug Synthesis”course to enrich the system for training talents in green pharmaceutical synthesis.In this experiment,carbon rod as anode,platinum sheet as cathode,tetrabutylammonium acetate as electrolyte,4-methylstyrene and amine thiocyanate were electrolyzed with 8 mA constant current in a three-neck bottle filled with acetonitrile under argon for 3.5 hours to give the target product in 68%isolated yield.This experiment includes the construction and debugging of electrolysis device,argon gas protection,monitoring of the reaction process,column chromatography,and NMR characterization of product.This teaching experiment,with its inexpensive,readily available raw materials,easy operation,safety,and short duration,is conducted using a blended online and offline teaching approach,which could serve as a widely applicable teaching experiment to enhance students'skills in organic electrochemical theory and experimental operations.

关 键 词：实验教学设计 药物合成 有机电合成 4-甲基苯乙烯 双硫氰基化反应 

分 类 号：TQ[化学工程]