School of Chemistry, Damghan University, Damghan 36715-364, Iran.
Acta Chim Slov. 2022 Jun 14;69(2):271-280. doi: 10.17344/acsi.2021.6761.
In this research, a novel magnetic nanocatalyst based on iron oxide nanoparticles linked with pyridinium hydrotribromide (Fe3O4@PyHBr3) was synthesized in three steps. In the first step, 3-(aminopropyl)triethoxysilane (APTES) was reacted with 4-(bromomethyl)pyridine hydrobromide. In the second step, the product obtained in the first step was reacted with iron oxide nanoparticles. In the last step, a grinding reaction was carried out with KBr and HIO4 in a mortar. The Fe3O4@PyHBr3 nanocatalyst was characterized by FT-IR, CHN, XRD, SEM, TGA and VSM analysis. The magnetic nanocatalyst was used as a catalyst for the selective oxidation of alcohols to aldehydes and ketones using 30% H2O2 as oxidant in a short time and with high yields. Moreover, no overoxidation of the alcohols was observed. The nanocatalyst was efficiently recycled in five consecutive cycles without significant loss of its catalytic activity. Moreover, trimethylsilylation and tetrahydropyranylation of alcohols were carried out in the presence of this nanocatalyst.
在这项研究中,通过三步合成了一种新型磁性纳米催化剂,其基于与氢溴酸吡啶(Fe3O4@PyHBr3)相连的氧化铁纳米粒子。在第一步中,3-(氨丙基)三乙氧基硅烷(APTES)与 4-(溴甲基)吡啶氢溴酸盐反应。在第二步中,第一步得到的产物与氧化铁纳米粒子反应。在最后一步,在研钵中用 KBr 和 HIO4 进行研磨反应。通过 FT-IR、CHN、XRD、SEM、TGA 和 VSM 分析对 Fe3O4@PyHBr3 纳米催化剂进行了表征。该磁性纳米催化剂在 30% H2O2 作为氧化剂的条件下,在短时间内高收率地选择性氧化醇为醛和酮,且无醇过度氧化现象。此外,该纳米催化剂在五次连续循环中可有效地回收,且催化活性无明显损失。此外,在该纳米催化剂的存在下还进行了醇的三甲基硅烷化和四氢吡喃化反应。