摘要
以2-氯异烟酸甲酯和2,4-双(甲氧羰基)苯硼酸片呐醇酯为原料,通过两步法合成了一种新颖的含吡啶基团的半刚性三元羧酸配体,采用核磁共振氢谱、红外光谱对配体结构进行了表征,并通过正交实验优化了配体单晶的培养条件。结果表明,在温度为140℃、时间为12 h、用50μL 0.24 mol·L^(-1)盐酸调节pH值、溶剂为5 mL乙醇的培养条件下,可得到最佳质量的半刚性三元羧酸配体单晶;该配体晶体属于单斜晶系,P2_(1/c)空间群,配体中裸露的6个氧原子及1个氮原子可以为金属离子的配位提供足够的位点。
Taking 2-chloropyridine-4-carboxylic acid tert-butyl ester and 2,4-bis(methoxycarbonyl)phenylboronic acid pinacol ester as raw materials,we synthesized a novel semi-rigid tricarboxylic acid ligand containing pyridine group by a two-step method,and characterized its structure by 1HNMR and FTIR.Moreover,we optimized the culture conditions of the ligand single crystal by orthogonal experiments.The results show that the high quality of semi-rigid tricarboxylic acid ligand single crystal can be obtained under the conditions as follows:the temperature of 140℃,the time of 12 h,50μL 0.24 mol·L^(-1) hydrochloric acid is adopted to adjust the pH value,and 5 mL ethanol is adopted as the solvent.The ligand crystal belongs to the monoclinic system with P2_(1/c) space group.The exposed six oxygen atoms and one nitrogen atom in the ligand can provide enough sites for the coordination of metal ions.
作者
尚坤
赵乐
高艺欣
王力彬
岳昌武
SHANG Kun;ZHAO Le;GAO Yixin;WANG Libin;YUE Changwu(Yan'an University,Yan'an 716000,China;Shaanxi Energy Institute,Xianyang 712000,China)
出处
《化学与生物工程》
CAS
2022年第12期51-54,64,共5页
Chemistry & Bioengineering
基金
陕西省教育厅基金项目(21JK0996)
延安大学科研项目(2019-17,YDQ2020-04)。
关键词
半刚性
三元羧酸配体
单晶培养
semi-rigid
tricarboxylic acid ligand
single crystal culture
