一种苯并[口恶]嗪衍生物的合成及晶体结构  

Synthesis and crystal structure of benzoxazine derivatives

作　　者：朱周静 张翠亚 高艳蓉 唐文强 ZHU Zhou-jing;ZHANG Cui-ya;GAO Yan-rong;TANG Wen-qiang(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：《精细与专用化学品》2024年第6期44-46,53,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);咸阳市分子影像与药物合成重点实验室项目(2021QXNL-PT-0008)。

摘　　要：报道了一种结构新颖的苯并[口恶]嗪衍生物——1-[2,6-二氯-4-(3,5-二甲基异[口恶]唑-4-基)苯基]-1,2-二氢-4H-苯并[d][1,3][口恶]嗪-4-酮(化合物3)的合成及晶体结构。在碳酸钾碱性条件下,2-{[2,6-二氯-4-(3,5-二甲基异[口恶]唑-4-基)苯基]氨基}苯甲酸(化合物1)与二溴甲烷(化合物2)发生关环反应得到化合物3。优化关环反应,结果表明:在以碳酸钾为碱、物料比n(化合物2)∶n(化合物1)=3.0∶1、在110℃下回流反应8h,产物化合物3的收率达到71.3%(以化合物1计)。化合物3的晶体结构经XRD单晶衍射表征。The synthesis and crystal structure of a novel benzoxazine derivative,1-(2,6-dichloro-4-(3,5-dimethylisoxazol-4-yl)phenyl)-1,2-dihydro-4H-benzo[d][1,3]oxazin-4-one(compound 3)was reported.The benzoxazine derivative(compound 3)was synthesized by ring-closing reaction of 2-((2,6-dichloro-4-(3,5-dimethylisoxazol-4-yl)phenyl)amino)benzoic acid(compound 1)with dibromomethane(compound 2)in the alkaline condition of potassium carbonate.It was found that the yield of the product compound 3 was 71.3%at 11o℃for 8h with potassium carbonate as base and the mole ratio of n(compound 2):n(compound 1)=3.0:1.The crystal structure of the product was characterized by XRD single crystal diffraction.

关 键 词：苯并[口恶]嗪衍生物 关环反应 合成 单晶结构 

分 类 号：TQ463[化学工程—制药化工]