双(5-溴吡啶-2-基)胺的合成研究  

Synthesis of bis(5-bromopyridin-2-yl)amine

作　　者：李晓花[1] 赵欣[1] 唐静[1] 王艳娇[1,2] LI Xiao-hua;ZHAO Xin;TANG Jing;WANG Yan-jiao(School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xianyang 712046,China;Xianyang Key Laboratory of Molecular Imaging and Drug Synthesis,Xianyang 712046,China)

机构地区：[1]陕西国际商贸学院医药学院,陕西咸阳712046 [2]咸阳市分子影像与药物合成重点实验室,陕西咸阳712046

出　　处：《化学工程师》2023年第8期10-13,共4页Chemical Engineer

基　　金：陕西省教育厅2022年度一般专项科研计划项目(22JK0276);咸阳市分子影像与药物合成重点实验室项目(2021QXNL-PT-0008)。

摘　　要：报道一种吡啶衍生物双(5-溴吡啶-2-基)胺(1)的合成。在NaH碱性作用下,5-溴吡啶-2-胺(2)和5-溴-2-氟吡啶(3)发生芳基亲核取代反应得到目标化合物(1),其结构经^(1)H_(NMR)、^(13)C_(NMR)和MS表征。并考察了影响产物(1)收率的主要因素,确定适宜的反应条件为:NaH的用量为n(NaH)∶n_((2))=1.5∶1、物料比为n_((3))∶n_((2))=1.2∶1、反应溶剂为四氢呋喃、25℃反应4h。在该条件下,产物(1)收率达到59.7%(以化合物(2)计)。The synthesis of bis(5-bromopyridin-2-yl)amine(1)is reported.Under the basic conditions of sodium hydride,the target compound(1)was obtained by the aryl nucleophilic substitution reaction of 5-bromopyridin-2-amine(2)and 5-bromo-2-fluoropyridine(3).The structure was characterized by^(1)H_(NMR),^(13)C_(NMR)and MS.Also,the main factors affecting the yield of product(1)were investigated,and the suitable reaction conditions were determined as follows:the amount of sodium hydride was n(NaH)∶n_((2))=1.5∶1,the material ratio was n_((3))∶n_((2))=1.2∶1,the reaction solvent was tetrahydrofuran,and the reaction was at 25℃for 4 hours.Under this conditions,the yield of product(1)reached 59.7%(calculated by compound(2)).

关 键 词：吡啶衍生物 芳基亲核取代反应 条件优化 

分 类 号：TQ463[化学工程—制药化工]