摘要
以2-氯异烟酸甲酯、2,5-双(甲氧羰基)苯硼酸片呐醇酯为原料,通过两步合成法制备一种新颖的含吡啶基团的三元羧酸配体。采用傅里叶变换红外光谱及热重分析对配体结构及热稳定性进行测试。通过溶剂热法对配体的单晶进行培养,考察反应温度、时间、pH值、溶剂等条件对单晶培养的影响。结果表明,在反应时间为24 h,无水乙醇做溶剂,反应温度160℃,反应pH=4时,可以获得大块晶体。X-射线单晶衍射结果证明该配体为单斜晶系,P 21/n空间群。该配体中含有六个氧原子,一个氮原子,可以为结构多样配合物的制备提供配体选择,有望应用于配合物的设计应用与吸附、催化等多种场景。
A novel tricarboxylic acid ligand containing pyridine group was synthesized from methyl 2-chloro-isonicotinate and 2,5-bis(methoxycarbonyl) phenylboronic acid pinacol ester by a two-step method.The structure and thermal stability of the ligands were characterized by Fourier transform infrared spectroscopy and thermogravimetric analysis.Then the ligand single crystal was grown by solvothermal method, and the effects of reaction temperature, time, pH value, solvent and other conditions on the single crystal growth were investigated.The results showed that when the reaction time was 24 h, absolute ethyl alcohol was used as solvent, the reaction temperature was 160 ℃,and the pH value was 4,the bulk crystals could be obtained.X-ray single crystal diffraction results show that the ligand is monoclinic, space group P 21/n.The ligand contains six oxygen atoms and one nitrogen atom, which can provide ligand selection for the preparation of complexes with various structures and is expected to be applied to various scenarios such as the design of complexes, adsorption and catalysis.
作者
尚坤
高艺欣
赵乐
孙瑞
王力彬
岳昌武
Shang Kun;Gao Yixin;Zhao Le;Sun Rui;Wang Libin;Yue Changwu(Yan’an University,Yan’an 716000,Shaanxi,China;Shaanxi Energy Institute,Xi’an 712000,Shaanxi,China)
出处
《工业催化》
CAS
2023年第2期52-56,共5页
Industrial Catalysis
基金
陕西省科技厅项目(2023-JC-QN-0930)
延安大学项目(YDQ2020-04,YDQ2019-17)。
关键词
催化化学
吡啶
三元羧酸
单晶结构
catalytic chemistry
pyridine
tricarboxylic acids
single crystal structure
