Hayes Maria T, Subanbekova Aizhamal, Andaloussi Yassin H, Eaby Alan C, Zaworotko Michael J
Department of Chemical Sciences, Bernal Institute, University of Limerick, Limerick V94 T9PX, Republic of Ireland.
Cryst Growth Des. 2024 Dec 25;25(2):444-451. doi: 10.1021/acs.cgd.4c01606. eCollection 2025 Jan 15.
Solid-state synthesis is an approach to organic synthesis that is desirable because it can offer minimal or no solvent waste, high yields, and relatively low energy footprints. Herein, we report the solid-state synthesis of a novel Schiff base, 4-{()-[(4-methylpyridin-3-yl)imino]methyl}benzoic acid (), synthesized through the reaction of an amine and an aldehyde. was prepared via solvent-drop (water) grinding (SDG) on a multigram scale with 97% yield and was characterized using FTIR, H NMR, and SCXRD. The pyridyl and carboxylate moiety present in make it suitable for use as a linker ligand and indeed was found to coordinate with Cu(II), Zn(II), and Cd(II) cations, enabling it to serve as a linker ligand for the assembly of coordination polymers. thereby formed 1D (spiro chain) and 2D (square lattice, , topology) coordination polymers via solvent-induced (layering or slurry) methods. The resulting coordination polymers were characterized though X-ray diffraction (SCXRD, PXRD) and TGA, further demonstrating the utility of green synthesis methods for the preparation of some classes of new linker ligands that can in turn be used for the preparation of coordination polymers.
固态合成是一种有机合成方法，它具有诸多优点，因为它能产生极少或无溶剂浪费、高产率以及相对较低的能源足迹。在此，我们报道了一种新型席夫碱4-{()-[(4-甲基吡啶-3-基)亚氨基]甲基}苯甲酸（）的固态合成，该席夫碱是通过胺与醛的反应合成的。通过溶剂滴加（水）研磨（SDG）以多克规模制备了该化合物，产率为97%，并使用傅里叶变换红外光谱（FTIR）、核磁共振氢谱（H NMR）和单晶X射线衍射（SCXRD）对其进行了表征。该化合物中存在的吡啶基和羧酸盐部分使其适合用作连接配体，实际上发现它能与铜（II）、锌（II）和镉（II）阳离子配位，从而使其能够作为连接配体用于组装配位聚合物。通过溶剂诱导（分层或淤浆）方法，由此形成了一维（螺旋链）和二维（方形晶格，，拓扑结构）配位聚合物。通过X射线衍射（SCXRD、粉末X射线衍射（PXRD））和热重分析（TGA）对所得配位聚合物进行了表征，进一步证明了绿色合成方法在制备某些新型连接配体方面的实用性，这些连接配体进而可用于制备配位聚合物。
