2,2′-(肼-1,2-二亚甲基)(2Z,2′Z)-双(2-苯乙酸)二甲酯的合成及晶体结构  

Synthesis and crystal structure of dimethyl 2,2′-(hydrazine-1,2-diylidene)(2Z,2′Z)-bis(2-phenylacetate)

作　　者：杜漠 赵梅梅 王一寓 党小琳[1] DU Mo;ZHAO Mei-mei;WANG Yi-yu;DANG Xiao-lin(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11期43-46,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)。

摘　　要：报道了2,2′-(肼-1,2-二亚甲基)(2Z,2′Z)-双(2-苯乙酸)二甲酯(化合物2)的合成方法及单晶结构。在二聚醋酸铑(Ⅱ)的催化作用下,2-重氮基-2-苯基乙酸乙酯(化合物1)发生分子间氮-氢键插入反应得到目标化合物2。优化并确定适宜的反应条件为n[二聚醋酸铑(Ⅱ)]∶n(化合物1)=0.05∶1、反应溶剂为甲苯、反应时间2h,在该条件下,化合物2的收率达到81.4%(以化合物1计)。产物结构经过ESI-MS及XRD单晶衍射表征。The synthesis and single crystal structure of dimethyl 2,2′-(hydrazine-1,2-diylidene)(2Z,2′Z)-bis(2-phenylacetate)(compound 2) was reported.The target compound 2 was obtained by intermolecular nitrogen-hydrogen bond insertion reaction of 2-diazo-2-phenyl ethyl acetate(compound 1) catalyzed by rhodium(Ⅱ) acetate dimer.The optimum reaction conditions were determined as follows:n[rhodium(Ⅱ) acetate dimer]∶n(compound 1)=0.05∶1,the reaction solvent was toluene,and the reaction time was 2 h,under this condition,the yield of compound 2 was up to 81.4%(calculated as compound 1).The structure of the product was characterized by ESI-MS and XRD single crystal diffraction.

关 键 词：肼类化合物 金属卡宾 氮-氢键插入反应 单晶衍射 

分 类 号：TQ463[化学工程—制药化工]