摘要
报道一种结构新颖的β-咔啉衍生物——1-苯基-9H-吡啶并[3,4-b]吲哚-3-羧酸甲酯(化合物2)的合成方法及单晶结构。在[1,1′-双(二苯基膦基)二茂铁]二氯化钯[Pd(dppf)Cl_(2)]催化作用下,3-氯-1-苯基-9H-吡啶并[3,4-b]吲哚(化合物1)在甲醇溶液中与一氧化碳发生插羰反应得到化合物2。优化并确定化合物2的最佳反应条件为:Pd(dppf)Cl_(2)用量为n[Pd(dppf)Cl_(2)]∶n(化合物1)=0.06∶1、反应在60℃下进行3h,化合物2的收率达到71.4%(以化合物1计)。化合物2的结构经过ESI-MS及XRD单晶衍射表征。
The synthesis and single crystal structure of a novelβ-carboline derivative methyl 1-phenyl-9Hpyrido[3,4-b] indole-3-carboxylate(compound 2)was reported.Compound 2 was obtained by carbonylation reaction of compound 1 with carbon monoxide in methanol solution by using Pd(dppf)Cl_(2) as the catalyst.Then,the reaction conditions were optimized and determined as follows:the amount of Pd(dppf)Cl_(2) used is n[Pd(dppf)Cl_(2)]:n(compound 1)=0.06:1,and the reaction is carried out at 60℃for 3 h,the yield of compound 2 reached 71.4%(based on compound 1).The structure of compound 2 was characterized by ESI-MS and XRD singlecrystal diffraction.
作者
杨新云
王睿函
仝红娟
YANG Xin-yun;WANG Rui-han;TONG Hong-juan(Xianyang Key Laboratory of Molecular Imaging and Drug Synthesis,School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xianyang 712046,China)
出处
《精细与专用化学品》
2025年第8期34-37,共4页
Fine and Specialty Chemicals
基金
咸阳市分子影像与药物合成重点实验室项目(2021QXNL-PT-0008)。
关键词
β-咔啉衍生物
插羰反应
条件优化
单晶衍射
β-carboline derivatives
carbonyl insertion reaction
condition optimization
single crystal diffraction
作者简介
杨新云(2004-),男,药学专业在读本科生;通讯作者:仝红娟(1989-),女,副教授,博士,研究方向为药物设计、合成及工艺研究。
