2,6-二氯-1,5-萘啶的合成研究  

Synthesis of 2,6-dichloro-1,5-naphnthyridine

作　　者：张瑞瑞[1,2] 朱周静 陈革豫 张彦民 刘斌 ZHANG Rui-rui;ZHU Zhou-jing;CHEN Ge-yu;ZHANG Yan-min;LIU Bin(School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xi'an 712046,China;Collaborative Innovation Center of Green Manufacturing Technology for Traditional Chinese Medicine in Shaanxi Province,Xi'an 712046,China)

机构地区：[1]陕西国际商贸学院医药学院,陕西西安712046 [2]陕西省中药绿色制造技术协同创新中心,陕西西安712046

出　　处：《精细与专用化学品》2020年第3期32-35,共4页Fine and Specialty Chemicals

基　　金：陕西国际商贸学院“中药药效物质研究”创新团队资助项目(SSY18TD01)。

摘　　要：以1,5-萘啶为原料,经过氧化反应得到1,5-萘啶-N-氧化物,1,5-萘啶-N-氧化物再经过氯代反应得到2,6-二氯-1,5-萘啶。其中间体及产物结构经1HNMR和ESI-MS确证。分别对两步反应中影响产物收率的因素进行了考察,确定的最佳氧化反应条件为:n(间氯过氧苯甲酸)∶n(1,5-萘啶)=3.5∶1,反应温度为25℃,反应时间为10h。最佳氯代反应条件为:反应温度为110℃,反应时间为30min。2,6-Dichloro-1,5-naphnthyridine was synthesized by a two-step reaction in 45%yield from 1,5-naphnthyridine through oxidation reaction and chlorination reaction.The structure of the product was confirmed by 1HNMR and ESI-MS.The optimal reaction conditions of two steps were also investigated respectively,and the optimal conditions of chlorination were as follows:n(m-CPBA)∶n(1,5-naphnthyridine)=3.5∶1,25℃for 10 h.The optimal conditions of oxidation were as follows:110℃for 30 min.

关 键 词：萘啶衍生物 1 5-萘啶 氧化反应 氯代反应 合成 

分 类 号：TQ463[化学工程—制药化工]