3-吲哚甲醛类衍生物的微通道反应器合成研究  

Synthetic Research of Indole-3-Carbonyl Compounds in Microchannel Reactor

作　　者：柯德宏 张文 吴孝兰 颜轲 许胜[2] KE De-hong;ZHANG Wen;WU Xiao-lan;YAN Ke;XU Sheng(Sinopharm Chemical Reagent Co.,Ltd,Shanghai 200002,China;School of Chemistry and Molecular Engineering,East China University of Science and Technology,Shanghai 200237,China)

机构地区：[1]国药集团化学试剂有限公司,上海200002 [2]华东理工大学化学与分子工程学院,上海200237

出　　处：《化学试剂》2023年第9期146-153,共8页Chemical Reagents

基　　金：国家自然科学基金项目(22071055)。

摘　　要：3-吲哚甲醛类化合物是非常重要的有机合成中间体,具有生理活性和药理活性,它在天然产物合成以及骨架构建中具有广泛应用。采用液-液混合进样方式,在连续流操作下使用微通道反应器合成14个3-吲哚甲醛类衍生物,所有产物都进行了表征,确认了分子结构。与实验室釜式条件相比,相同条件下(配比、温度、时间、溶剂等)使用微通道反应器合成,产物产率几乎不变,反应速率明显提高,反应时间从1.5 h缩短为54 s,反应容量扩大,从毫克级别扩大到公斤级,反应温度从45℃降至室温,这表明,微通道反应器有效克服了釜式反应器间歇工艺存在的反应效率低、传质传热不高、产率低等缺点,为以后连续化生产提供了工艺条件。Indole-3-formaldehyde compounds are very important organic intermediates,with physiological activity and pharmacological activities.It is widely used in natural product synthesis and bone architecture construction.In this paper,fourteen indole-3-formaldehyde derivatives were synthesized using a microchannel reactor using a liquid-liquid mixed injection method under continuous flow operation,and all products were characterized.Compared with the laboratory kettle test conditions,using a microchannel reactor under the same conditions(ratio,temperature,time,solvent,etc.)resulted in almost no change in product yield,and the reaction rate has significantly increased,the reaction time has been shortened from 1.5 h to 54 s,the reaction capacity has expanded from milligrams to kilograms,and the reaction temperature had decreased from 45℃to room temperature.Our result indicated that the microchannel reactor effectively overcomes the shortcomings of low reaction efficiency and low heat transfer in the intermittent process of the kettle reactor,our work provided the process conditions for future continuous production.

关 键 词：吲哚羰基类化合物 微通道反应器 连续流 甲酰化 公斤级 

分 类 号：O65[理学—分析化学]