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)

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.