N-[4′-氯-(1,1′-联苯)-2-基]甲酰胺的 合成及晶体结构  

Synthesis and crystal structure of N-(4′-chloro-(1,1′-biphenyl)-2-yl)formamide

作　　者：杜漠 赵梅梅 王一寓 唐文强 DU Mo;ZHAO Mei-mei;WANG Yi-yu;TANG Wen-qiang(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4期31-33,共3页Fine and Specialty Chemicals

基　　金：陕西省教育厅专项科研计划项目(22JK0277);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N-[4′-氯-(1,1′-联苯)-2-基]甲酰胺(化合物2)的合成方法及单晶结构。在N-丁基咪唑三氟乙酸盐离子液体催化下,4′-氯-(1,1′-二苯基)-2-胺(化合物1)与甲酸发生缩合反应得到产物化合物2。优化并确定的最佳反应条件为:甲酸与化合物1物质的量比为1.4:1,反应在75℃下进行1h,化合物2收率达到88.4%(以化合物1计)。化合物2结构经过ESI-MS及XRD单晶衍射表征。The synthesis and crystal structure of N-(4′-chloro-(1,1′-biphenyl)-2-yl)formamide(compound 2)was synthesized by condensation of 4′-chloro-(1,1′-diphenyl)-2-amine(compound 1)with formic acid catalyzed by N-butyl imidazole trifluoroacetate ionic liquid.Then the reaction conditions were optimized and determined as follows:the molar ratio of formic acid to compound 1 was 1.4:1,reaction temperature was 75℃,reaction time was lh.Under these conditions,the yield of compound 2 reached 88.4%(based on compound 1).The structure of the compound 2 was characterized by ESI-MS and XRD single crystal diffraction.

关 键 词：离子液体 缩合反应 条件优化 单晶衍射 

分 类 号：TQ463[化学工程—制药化工]