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负载于磁铁矿上的锑物种:一种用于将硝基芳烃直接进行克级规模还原偶联为偶氮芳烃的新型高效磁可重复使用纳米催化剂。

Immobilized antimony species on magnetite: a novel and highly efficient magnetically reusable nanocatalyst for direct and gram-scale reductive-coupling of nitroarenes to azoarenes.

作者信息

Zeynizadeh Behzad, Faraji Fariba

机构信息

Faculty of Chemistry, Urmia University Urmia 5756151818 Iran

出版信息

RSC Adv. 2019 Apr 29;9(23):13112-13121. doi: 10.1039/c9ra01249d. eCollection 2019 Apr 25.

Abstract

In this study, magnetic nanoparticles of FeO@SbF from the immobilization of SbF on magnetite were synthesized. The prepared nanocomposite system was then characterized using scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, energy-dispersive X-ray spectroscopy, vibrating sample magnetometry and inductively coupled plasma optical emission spectroscopy. Next, the catalytic activity of FeO@SbF MNPs was highlighted by one-pot reductive-coupling of aromatic nitro compounds to the corresponding azoarene materials with NaBH. The reactions were carried out in refluxing EtOH within 6-25 min to afford the products in high yields. The reusability of the Sb-magnetite system was also studied for 6 consecutive cycles without significant loss of catalytic activity. This synthetic protocol provided several advantages in terms of introducing a novel catalytic system based on antimony species for direct and gram-scale preparation of azoarenes from nitroarenes, low loading of the nanocatalyst, mild reaction conditions, using ethanol as a green and economic solvent and high yield of the products.

摘要

在本研究中,通过将SbF固定在磁铁矿上合成了FeO@SbF磁性纳米颗粒。然后使用扫描电子显微镜、傅里叶变换红外光谱、X射线衍射、能量色散X射线光谱、振动样品磁强计和电感耦合等离子体发射光谱对制备的纳米复合体系进行表征。接下来,通过用NaBH将芳香族硝基化合物一锅法还原偶联为相应的偶氮芳烃材料,突出了FeO@SbF磁性纳米颗粒的催化活性。反应在回流乙醇中进行6 - 25分钟,以高产率得到产物。还对Sb - 磁铁矿体系的可重复使用性进行了连续6个循环的研究,其催化活性没有明显损失。该合成方案在引入基于锑物种的新型催化体系以直接从硝基芳烃大规模制备偶氮芳烃方面具有多个优点,包括纳米催化剂负载量低、反应条件温和、使用乙醇作为绿色经济溶剂以及产物收率高。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d505/9063975/521ffa436efa/c9ra01249d-s1.jpg

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