[2-(4-溴-2,6-二氯苯氨基)苯基]吗啉甲酮的合成及晶体结构  

Synthesis and crystal structure of (2-((4-bromo-2,6-dichlorophenyl)amino)phenyl)(morpholino)methanone

作　　者：王艳娇[1] 张翠亚 郑浩亮 唐文强 朱周静 WANG Yan-jiao;ZHANG Cui-ya;ZHENG Hao-liang;TANG Wen-qiang;ZHU Zhou-jing(Xianyang Key Laboratory of Molecular Imaging and Drug Synthesis,School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xianyang 712046,China)

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

出　　处：《精细与专用化学品》2024年第9期43-45,55,共4页Fine and Specialty Chemicals

基　　金：陕西省教育厅专项科研计划项目(23JK0323);咸阳市分子影像与药物合成重点实验室项目(2021QXNL-PT-0008);陕西国际商贸学院中药药效物质研究创新团队建设项目。

摘　　要：报道一种邻氨基苯甲酰胺衍生物——[2-(4-溴-2,6-二氯苯氨基)苯基]吗啉甲酮(化合物3)的合成及单晶结构。在缩合剂2-(7-氮杂苯并三氮唑)-N,N,N′,N′-四甲基脲六氟磷酸酯(HATU)作用下,2-[(4-溴-2,6-二氯苯基)氨基]苯甲酸(化合物1)与吗啡啉(化合物2)发生缩合反应得到化合物3。反应条件优化结果表明:当物料比n(化合物2)∶n(化合物1)=1.3∶1、N,N-二甲基甲酰胺为反应溶剂,在40℃条件下反应2h,化合物3的收率达到88.2%(以化合物1计)。采用XRD单晶衍射对化合物3的晶体结构进行表征,发现晶体结构属于单斜晶系,P2_(1)/c空间群。The synthesis and single crystal structure of(2-((4-bromo-2,6-dichlorophenyl)amino)phenyl)(morpholino)methanone(compound 3),a derivative of o-aminobenzamide was reported.Under the action of condensation agent 2-(7-Azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate(HATU),2-((4-bromo-2,6-dichlorophenyl)amino)benzoic acid(compound 1) reacted with morpholine(compound 2) to yield the product(compound 3).The results showed that the yield of the product was 88.2%(calculated as compound 1) when n(compound 2)∶n(compound 1)=1.3∶1,N,N-dimethylformamide was used as the solvent and the reaction condition was 40℃ for 2h.The crystal structure of the product was characterized by XRD single crystal diffraction.It was found that the crystal structure of the product belongs to monoclinic crystal system, P2_(1)/c space group.

关 键 词：邻氨基苯甲酰胺衍生物 缩合反应 条件优化 单晶衍射 

分 类 号：TQ463[化学工程—制药化工]