2-{[4-(3,5-二甲基异唑-4-基)-2,6-二氟苯基]氨基}苯甲酸乙酯的合成及晶体结构  

Synthesis and crystal structure of ethyl 2-((4-(3,5-dimethylisoxazol-4-yl)-2,6-difluorophenyl)amino)benzoate

作　　者：党小琳[1] 张凯[2] 赵欣[1] 李晓花[1] 唐文强 DANG Xiao-lin;ZHANG Kai;ZHAO Xin;LI Xiao-hua;TANG Wen-qiang(School of Pharmacy,Shaanxi Institute of International Trade&.Commerce,Xianyang 712046,China;Shaanxi Polytechnic Institute,Xianyang 712000,China)

机构地区：[1]陕西国际商贸学院医药学院,陕西咸阳712046 [2]陕西工业职业技术学院,陕西咸阳712000

出　　处：《精细与专用化学品》2024年第4期28-30,39,共4页Fine and Specialty Chemicals

基　　金：陕西省科技厅2023年重点研发计划项目(2023-YBSF-036);陕西省教育厅一般专项科研计划项目(22JK0279);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2-{[4-(3,5-二甲基异唑-4-基)-2,6-二氟苯基]氨基}苯甲酸乙酯(化合物1)的合成及晶体结构。在三乙胺碱性条件下,2-{[4-(2,4-二氧戊烷-3-基)-2,6-二氟苯基]氨基}苯甲酸乙酯(化合物2)与盐酸羟胺反应得到目标化合物1。考察并确定适宜的反应条件为:当反应溶剂为乙醇、物料比为n(盐酸羟胺):n(化合物2)=1.4:1、回流反应6h,产物化合物1的收率达到58.5%(以化合物2计)。通过质谱及XRD单晶衍射对产物结构进行表征。The synthesis and crystal structure of ethyl 2-((4-(3,5-dimethylisoxazol-4-yl)-2,6-difluorophenyl)amino)benzoate was reported.In the presence of triethylamine,the target compound(1)was obtained by the reaction of ethyl 2-((4-(2,4-dioxopentan-3-yl)-2,6-difluorophenyl)amino)benzoate(compound(2))with hydroxylamine hydrochloride.The optimum reaction conditions were determined as follows:when the reaction solvent was ethanol,the mole ratio of NH,OH·HCl and compound(2)was 1.4:l,and the reflux reaction was carried out for 6 hours,the yield of the product was 58.5%(calculated as compound(2)).The structure of the product was characterized by mass spectrometry and XRD Single Crystal Diffraction.

关 键 词：异唑衍生物 合成 条件优化 单晶结构 

分 类 号：TQ463[化学工程—制药化工]