Comparative study of catalytic performance of TiP and Ti-ATMP towards dihydropyrimidinones synthesis

IF 2.8 3区化学 Q2 CHEMISTRY, MULTIDISCIPLINARY

Research on Chemical Intermediates Pub Date : 2025-05-11 DOI:10.1007/s11164-025-05594-5

Mithil Kevadiya, Kalpana Maheria

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Abstract

In the present research, inorganic titanium phosphate (TiP) and hybrid titanium-aminotrismethylene phosphonic acid (Ti-ATMP) materials, belonging to the class of tetravalent metal acid (TMA) salts, have been synthesized via the sol–gel route. These materials have been characterized by high-angle X-ray diffraction (HXRD), thermogravimetric analysis (TGA), Fourier transforms infrared spectroscopy (FT-IR), scanning electron microscopy-energy dispersive X-ray analysis (SEM–EDX), X-ray photoelectron spectroscopy (XPS), High resolution-transmission electron microscopy (HR-TEM), N₂ sorption isotherms and evaluation of surface acidity via the temperature programmed desorption (NH₃-TPD) method. Due to the presence of exchangeable protons in the framework of TiP and Ti-ATMP materials, they can act as solid acid catalysts and hence an attempt has been made for the catalyzed synthesis of dihydropyrimidinones (DHPMs) using these materials. The effects of reaction time, temperature, catalyst concentration and substituents on DHPMs synthesis have been studied. Further, the reaction is carried out in various solvents and under solvent free conditions in order to evaluate the feasibility of developed protocol to be used under diverse chemical environment. The isolated DHPM products were characterized based on their physical melting point (M.P.), FT-IR, ¹H and ¹³C NMR spectroscopy. The recyclability and stability studies of the catalysts have been performed to assess their potential for reuse.

Graphical abstract

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TiP和Ti-ATMP对二氢嘧啶合成催化性能的比较研究

本研究采用溶胶-凝胶法制备了四价金属酸（TMA）盐类无机磷酸钛（TiP）和杂化钛-氨基三亚甲基膦酸（Ti-ATMP）材料。采用高角x射线衍射（HXRD）、热重分析（TGA）、傅里叶变换红外光谱（FT-IR）、扫描电子显微镜-能量色散x射线分析（SEM-EDX）、x射线光电子能谱（XPS）、高分辨率透射电子显微镜（HR-TEM）、N2吸附等温线和程序升温解吸法（NH3-TPD）对材料表面酸度进行了表征。由于TiP和Ti-ATMP材料框架中存在可交换质子，它们可以作为固体酸催化剂，因此人们尝试使用这些材料催化合成二氢嘧啶（dhpm）。研究了反应时间、反应温度、催化剂浓度和取代基对双聚苯胺合成的影响。此外，该反应在各种溶剂和无溶剂条件下进行，以评估所制定的方案在不同化学环境下使用的可行性。通过物理熔点（mp）、红外光谱（FT-IR）、1H和13C NMR对分离得到的DHPM产物进行了表征。对催化剂的可回收性和稳定性进行了研究，以评估其再利用潜力。图形抽象

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来源期刊

Research on Chemical Intermediates 化学-化学综合

CiteScore

5.70

自引率

18.20%

发文量

229

审稿时长

2.6 months

期刊介绍： Research on Chemical Intermediates publishes current research articles and concise dynamic reviews on the properties, structures and reactivities of intermediate species in all the various domains of chemistry. The journal also contains articles in related disciplines such as spectroscopy, molecular biology and biochemistry, atmospheric and environmental sciences, catalysis, photochemistry and photophysics. In addition, special issues dedicated to specific topics in the field are regularly published.