Bayzidi Massood, Zeynizadeh Behzad
Department of Chemistry, Urmia University Urmia 5756151818 Iran
RSC Adv. 2022 May 17;12(24):15020-15037. doi: 10.1039/d2ra02293a.
In this study, a crafted zirconocene complex on rGO@FeO as a novel magnetic nanocatalyst was synthesized and then characterized using FT-IR, SEM, EDX, VSM, ICP-OES, TGA, BET and MS analyses. Next, catalytic activity of the prepared nanocomposite rGO@FeO/ZrCpCl towards successful reduction of aromatic nitro compounds to arylamines using NH·HO (80%) was investigated. The examined nanocatalyst also showed perfect catalytic activity for reductive-acetylation of aromatic nitro compounds to the corresponding -arylacetamides without isolation of the prepared amines using the NH·HO/AcO system. Furthermore, acetylation of the commercially available arylamines to the corresponding -arylacetamides was carried out by acetic anhydride in the presence of the rGO@FeO/ZrCpCl nanocomposite. All reactions were carried out in refluxing EtOH as a green solvent to afford the products in high yields. The obtained results exhibited that the nanocomposite of rGO@FeO/ZrCpCl showed a great catalytic activity in comparison to rGO and rGO@FeO as the parent constituents. Recovery and reusability of rGO@FeO/ZrCpCl were also examined for 8 consecutive cycles without significant loss of the catalytic activity. This establishes the sustainable anchoring of the zirconocene complex on the surface and mesopores of the rGO@FeO nanohybrid system.
在本研究中,合成了一种负载于rGO@FeO上的精心设计的锆茂配合物作为新型磁性纳米催化剂,然后通过傅里叶变换红外光谱(FT-IR)、扫描电子显微镜(SEM)、能谱分析(EDX)、振动样品磁强计(VSM)、电感耦合等离子体发射光谱(ICP-OES)、热重分析(TGA)、比表面积分析(BET)和质谱分析(MS)对其进行了表征。接下来,研究了制备的纳米复合材料rGO@FeO/ZrCpCl使用水合肼(80%)将芳香族硝基化合物成功还原为芳胺的催化活性。所研究的纳米催化剂还表现出优异的催化活性,能够在不分离制备的胺的情况下,使用水合肼/醋酸体系将芳香族硝基化合物还原乙酰化为相应的芳基乙酰胺。此外,在rGO@FeO/ZrCpCl纳米复合材料存在下,通过乙酸酐将市售芳胺乙酰化为相应的芳基乙酰胺。所有反应均在作为绿色溶剂的回流乙醇中进行,以高产率得到产物。所得结果表明,与作为母体成分的rGO和rGO@FeO相比,rGO@FeO/ZrCpCl纳米复合材料表现出很高的催化活性。还对rGO@FeO/ZrCpCl进行了8个连续循环的回收和再利用测试,其催化活性没有明显损失。这证实了锆茂配合物在rGO@FeO纳米杂化体系表面和中孔上的可持续锚定。