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One-pot preparation of ZnO-SnO₂@rGO nanocomposite using Bougainvillea glabra flower extract and evaluation of its photocatalytic removal of Coomassie Brilliant Blue 九重葛花提取物一锅法制备ZnO-SnO 2 @rGO纳米复合材料及其光催化脱除考马斯亮蓝效果评价
IF 2.1 3区 化学 Q3 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2026-01-09 DOI: 10.1016/j.jorganchem.2026.124015
G.K. Ayyadurai , M.K. Raman , K. Selvaraju , Gunasekaran Somasundaram , Paulson Emerson
Discharging untreated and unmonitored dye waste poses a significant threat to the influential and thriving textile dyeing sectors of several countries. The rigid chemical bonding of that dye hinders its degradation, making photocatalytic processes a superior method for degrading industrial dyes. In the present work, zinc oxide (ZnO) and tin oxide (SnO₂) on reduced graphene oxide (rGO) nanosheets were prepared to produce a ZnO-SnO₂@rGO nanocomposite as a nano-photocatalyst via a simple, eco-friendly, one-pot green synthesis approach employing Bougainvillaea glabra flower extract (BGFE) as a green reducing agent. The synthesized ZnO-SnO₂@rGO nanocomposite was characterized through various analytical techniques, including XRD, FT-IR, UV‒Vis, SEM, and XPS. XRD analysis confirmed the formation of hexagonal wurtzite ZnO and tetragonal-phased SnO₂ nano-crystallites on rGO with a crystallite size of 2.19 nm. The optical bandgap was calculated and found to be in the photon energy range of 2.6 eV for the ZnO-SnO₂@rGO nanocomposite. Morphological analysis confirmed the formation of rod-shaped ZnO nanoparticles and spherical SnO₂ clusters anchored well onto the layered rGO sheets. The ability of the ZnO-SnO₂@rGO nanocomposite to degrade Coomassie Brilliant Blue R 250 (CBB R 250) dye under sunlight irradiation was examined. The ZnO-SnO₂@rGO nanocomposite effectively degraded 98.8% and 96.7% of the different dye dosages of CBB R 250 dye within 60 and 100 min under solar irradiation, respectively. The ZnO-SnO₂@rGO catalyst demonstrated reliable performance during seven consecutive cycles of reusability, and XRD examination further validated its structural stability.
排放未经处理和不受监测的染料废料对若干国家有影响力和蓬勃发展的纺织染色部门构成重大威胁。这种染料的刚性化学键阻碍了它的降解,使得光催化过程成为降解工业染料的一种优越方法。本研究以九重葛花提取物(BGFE)为绿色还原剂,在还原氧化石墨烯(rGO)纳米片上制备氧化锌(ZnO)和氧化锡(SnO₂)作为纳米光催化剂,采用简单、环保、一锅绿色合成的方法制备ZnO-SnO₂@rGO纳米复合材料。通过XRD、FT-IR、UV-Vis、SEM和XPS等分析技术对合成的ZnO-SnO 2 @rGO纳米复合材料进行了表征。XRD分析证实在氧化石墨烯上形成了六方纤锌矿ZnO和四方相sno2纳米晶,晶粒尺寸为2.19 nm。计算结果表明,ZnO-SnO 2 @rGO纳米复合材料的光学带隙在2.6 eV的光子能量范围内。形貌分析证实了棒状ZnO纳米粒子的形成和球形SnO₂团簇在层状氧化石墨烯薄片上锚定良好。考察了ZnO-SnO 2 @rGO纳米复合材料在日光照射下对考马斯亮蓝r250 (CBB r250)染料的降解能力。在太阳照射下,ZnO-SnO 2 @rGO纳米复合材料分别在60 min和100 min内有效降解了98.8%和96.7%的不同染料用量的CBB r250染料。ZnO-SnO 2 @rGO催化剂在连续7次循环使用中表现出可靠的性能,XRD测试进一步验证了其结构稳定性。
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引用次数: 0
The synthesis of (η6-arene)tricarbonylchromium complexes of dihydro derivatives of 1,3- and 1,4-benzoxazines 1,3-和1,4-苯并恶嗪二氢衍生物(η - 6-芳烃)三羰基铬配合物的合成
IF 2.1 3区 化学 Q3 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2026-01-07 DOI: 10.1016/j.jorganchem.2026.124012
Alexander V. Grishin , Elena V. Sazonova , Nikolay V. Somov , Svetlana V. Baryshnikova , Andrey Yu. Shishkin , Vasily F. Smirnov , Natalia Yu. Grishina
The series of new (η6-arene)tricarbonylchromium π-complexes were obtained by the reaction of 3-phenyl-3,4-dihydro-2Н-1,3-benzoxazine (1), 3,4-dihydro-2Н-1,4-benzoxazine (2) and 3-phenyl-3,4-dihydro-2Н-1,4-benzoxazine (3) with triammine(tricarbonyl)chromium (4) in refluxing dioxane. It was found out that in the case of the 1,3-benzoxazine ligand 1 the coordination of tricarbonylchromium group occurs via phenyl substituent. It was shown that processes involving 1,4-benzoxazine derivatives 2, 3 are characterized by coordination of tricarbonylchromium group on phenylene fragment. The novel compounds were characterized by UV–vis, IR, NMR spectroscopy, mass spectrometry, HPLC. The performed single-crystal X-ray diffraction studies confirmed the formation of complexes via η6-coordination of aromatic fragments of benzoxazine ligands by chromium atom.
通过3-苯基-3,4-dihydro-2Н-1,3-苯并恶嗪(1),3,4-dihydro-2Н-1,4-苯并恶嗪(2)和3-苯基-3,4-dihydro-2Н-1,4-苯并恶嗪(3)与三胺(三羰基)铬(4)在回流二恶烷中反应,得到了一系列新的(η - 6-芳烃)三羰基铬π配合物。结果表明,在1,3-苯并恶嗪配体1中,三羰基铬的配位是通过苯基取代基进行的。结果表明,涉及1,4-苯并恶嗪衍生物2,3的反应过程以三羰基铬基在苯基片段上的配位为特征。采用紫外可见光谱、红外光谱、核磁共振光谱、质谱、高效液相色谱等方法对化合物进行了表征。单晶x射线衍射研究证实了铬原子与苯并恶嗪配体芳香族片段通过η - 6配位形成配合物。
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引用次数: 0
Generation of the intramolecular hydrogen bonding of a parallel β-sheet nucleated by a rigid bimetallic ring 由刚性双金属环成核的平行β片分子内氢键的产生
IF 2.1 3区 化学 Q3 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2026-01-07 DOI: 10.1016/j.jorganchem.2026.124014
Timothy P. Curran , Alessandro Marrone , Iogann Tolbatov , Lilly L. Pubillones , Thanh T. Nguyen , Joanne Stewart
Two glycine residues were appended to two alkyne ligands in a rigid, bimetallic ring that features both a 1,1′-ferrocene and a tungsten bis-alkyne to yield complex 4a-b. The conformation of 4a-b was probed using NMR and computational methods. The results show that the bimetallic ring system holds the two glycine residues in a conformation similar to that found in a parallel β-sheet, and that this conformation is made robust by formation of four intramolecular hydrogen bonds. In contrast, a diester derivative, 13a-b, adopts a conformation where only one of the two NH protons are involved in an intramolecular hydrogen bond. The findings suggest that in 4a-b the bimetallic ring system adopts a nascent β-sheet conformation.
两个甘氨酸残基被附加到两个炔配体上,形成一个刚性的双金属环,该环具有1,1 ' -二茂铁和钨双炔,从而得到配合物4a-b。采用核磁共振和计算方法对4a-b的构象进行了探测。结果表明,双金属环体系将两个甘氨酸残基保持在一个类似于平行β-片的构象中,并且该构象通过形成四个分子内氢键而变得坚固。相反,二酯衍生物13a-b采用的构象是两个氢原子中只有一个参与分子内氢键。结果表明,在4a-b中,双金属环体系采用新生的β-薄片构象。
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引用次数: 0
High-yielding preparation of Diaryl ketones via carbonylative cross-coupling reactions using a magnetic/carbon nanotube supported palladium catalyst in DESs solvent 磁性/碳纳米管负载钯催化剂在DESs溶剂中羰基化交叉偶联反应高产制备二芳基酮
IF 2.1 3区 化学 Q3 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2026-01-03 DOI: 10.1016/j.jorganchem.2026.124010
Mohamed Abu Shuheil , Magdi E.A. Zaki , G. Padma Priya , Qusay Husam Aziz , Y. Sasikumar , Ahmed Aldulaimi , Renu Sharma , Sobhi M. Gomha , Mosstafa Kazemi
A novel heterogeneous palladium catalyst, MWCNTs/MNPs–TAEA–Phen–Pd(0), was developed and applied for the efficient synthesis of diaryl ketones via carbonylative Suzuki–Miyaura coupling reactions. The MWCNTs/MNPs–TAEA–Phen–Pd(0) catalyst integrates multi-walled carbon nanotubes (MWCNTs) and magnetic nanoparticles (Fe₃O₄) functionalized with tris(2-aminoethyl)amine (TAEA) and 1,10-phenanthroline (Phen) ligands, providing high dispersion and stabilization of Pd(0) species. Under optimized conditions, a wide variety of aryl iodides and arylboronic acids were successfully transformed into the corresponding diaryl ketones in excellent yields (79–98%), demonstrating broad substrate tolerance toward both electron-donating and electron-withdrawing substituents. The MWCNTs/MNPs–TAEA–Phen–Pd(0) catalyst exhibited outstanding recyclability, maintaining 90% yield after seven consecutive runs, as confirmed by SEM, FT-IR, XRD, ICP-OES and VSM analyses. Significant advantages of this system include high catalytic activity, easy magnetic separation, robust stability, and eco-friendly reaction conditions using a ChCl–glycerol solvent system. These results establish MWCNTs/MNPs–TAEA–Phen–Pd(0) as an efficient, durable, and magnetically separable nanocatalyst for sustainable carbonylative coupling reactions, providing a green and practical alternative to conventional homogeneous palladium systems.
制备了一种新型非均相钯催化剂MWCNTs/ MNPs-TAEA-Phen-Pd(0),并将其应用于羰基化Suzuki-Miyaura偶联反应中高效合成二芳基酮。MWCNTs/ MNPs-TAEA-Phen-Pd(0)催化剂集成了多壁碳纳米管(MWCNTs)和三(2-氨基乙基)胺(TAEA)和1,10-菲罗啉(Phen)配体功能化的磁性纳米颗粒(Fe₃O₄),提供了Pd(0)的高分散性和稳定性。在优化的条件下,多种芳基碘化物和芳基硼酸以优异的收率(79-98%)成功转化为相应的二芳基酮,对供电子和吸电子取代基都表现出广泛的底物耐受性。SEM、FT-IR、XRD、ICP-OES和VSM分析均证实,MWCNTs/ MNPs-TAEA-Phen-Pd(0)催化剂具有出色的可回收性,连续运行7次后收率仍保持90%。该体系具有催化活性高、易于磁分离、稳定性强、反应环境友好等优点。这些结果表明,MWCNTs/ MNPs-TAEA-Phen-Pd(0)是一种高效、耐用、可磁性分离的纳米催化剂,可用于可持续羰基化偶联反应,为传统的均相钯体系提供一种绿色实用的替代方案。
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引用次数: 0
Construction of MWCNTs/MNPs-based copper nanocomposite as an efficient and reusable catalyst for four-component preparation of highly substituted pyridines MWCNTs/ mnps基铜纳米复合材料高效可重复使用的四组分高取代吡啶制备催化剂的构建
IF 2.1 3区 化学 Q3 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2026-01-03 DOI: 10.1016/j.jorganchem.2026.124011
Mohamed Abu Shuheil , Ahmed Aldulaimi , Rekha MM , Subhashree Ray , Omayma Salim Waleed , CP. Surya , Renu Sharma , Vatsal Jain
A sustainable and highly efficient four-component protocol has been established for the synthesis of structurally diverse and highly substituted pyridine derivatives. The catalytic system, MWCNTs/MNPs–Tris(2-aminoethyl)amine–CuCl₂, effectively promotes the one-pot condensation of aromatic aldehydes, malononitrile, ethyl acetoacetate, and substituted anilines in aqueous medium under reflux conditions. This green catalytic method provides the desired pyridines in excellent yields (86–98%) within 1 h, highlighting its remarkable activity and selectivity. The reaction system exhibits wide substrate compatibility, tolerating both electron-donating and electron-withdrawing substituents on the aromatic rings. Product identity and purity were confirmed by melting-point determination and observation of crystalline or oily characteristics. A comparative evaluation with existing protocols demonstrates significant advantages in yield, environmental compatibility, and operational simplicity. The use of water as an environmentally benign solvent, along with the recyclable magnetic nanocatalyst, underscores the method's sustainability and reusability. Overall, this approach provides a green, rapid, and practical route to valuable pyridine-based heterocycles with potential biological relevance.
建立了一种可持续、高效的四组分方案,用于合成结构多样、高取代的吡啶衍生物。MWCNTs/ MNPs-Tris(2-氨基乙基)胺- cucl₂催化体系在回流条件下可有效促进芳香醛、丙二腈、乙酰乙酸乙酯和取代苯胺在水介质中的一锅缩合反应。该绿色催化方法在1 h内以86-98%的收率获得了理想的吡啶,突出了其良好的活性和选择性。该反应体系具有广泛的底物相容性,可耐受芳香环上的供电子和吸电子取代基。通过熔点测定和观察结晶或油性特征来确定产品的纯度。与现有方案的比较评估表明,在产量、环境兼容性和操作简单性方面具有显着优势。使用水作为环保溶剂,以及可回收的磁性纳米催化剂,强调了该方法的可持续性和可重复使用性。总的来说,这种方法提供了一条绿色、快速和实用的途径,可以获得具有潜在生物学意义的有价值的吡啶类杂环化合物。
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引用次数: 0
Self-assembly of half-sandwich iridium-based metallarectangles for the encapsulation of polycyclic aromatic hydrocarbons 半夹心铱基金属矩形的自组装封装多环芳烃
IF 2.1 3区 化学 Q3 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-12-30 DOI: 10.1016/j.jorganchem.2025.123998
Si Nian , Zhi-Yang Chen , Shou-You Jiao , Ming-Xin Liang , Yu-Fei Zhu , Chengzhu He , Xianghuan Shan , Wei-Long Shan
The rational design and synthesis of metallarectangles with tailored cavities and functionalities remain a formidable challenge in organometallic supramolecular chemistry. Here, we report two half-sandwich iridium-based metallarectangles, [Cp₂Ir₂Cl₂]₂L₂(OTf)₄ (1) and [Cp₂Ir₂(μ-DHBQ)]₂L₂(OTf)₄ (2), which were obtained in high yields via coordination-driven self-assembly of binuclear precursors B1 and B2 employing a 2,1,3-benzothiadiazole (BTD)-based bidentate ligand L. Based on single-crystal XRD analysis, the molecular structures of these complexes adopt tetranuclear rectangular macrocyclic architectures with cavities of distinct dimensions. Subsequent NMR titration studies confirmed that metallarectangle 2 exhibits exceptional host-guest properties, notably encapsulating electron-rich polycyclic aromatic hydrocarbons (PAHs) such as anthracene, phenanthrene, and pyrene. Additionally, the crystal structure of complex 2⊃pyrene provides molecular-level insight into the key interactions governing host-guest assembly and stability.
在有机金属超分子化学中,合理设计和合成具有定制腔体和功能的金属矩形仍然是一个艰巨的挑战。本文报道了以2,1,3-苯并噻唑(BTD)为基础的双齿配体L,通过配位驱动自组装双核前体B1和B2,以高收率制备了[Cp₂Ir₂Cl₂]₂L₂(OTf)₄(1)和[Cp₂Ir₂(μ-DHBQ)]₂L₂(OTf)₄(2)两种半夹心铱基金属矩形配合物。随后的核磁共振滴定研究证实,金属矩形2表现出特殊的主客体性质,特别是封装富电子的多环芳烃(PAHs),如蒽、菲和芘。此外,复合体2、芘的晶体结构提供了分子水平上对主客体组装和稳定性的关键相互作用的洞察。
{"title":"Self-assembly of half-sandwich iridium-based metallarectangles for the encapsulation of polycyclic aromatic hydrocarbons","authors":"Si Nian ,&nbsp;Zhi-Yang Chen ,&nbsp;Shou-You Jiao ,&nbsp;Ming-Xin Liang ,&nbsp;Yu-Fei Zhu ,&nbsp;Chengzhu He ,&nbsp;Xianghuan Shan ,&nbsp;Wei-Long Shan","doi":"10.1016/j.jorganchem.2025.123998","DOIUrl":"10.1016/j.jorganchem.2025.123998","url":null,"abstract":"<div><div>The rational design and synthesis of metallarectangles with tailored cavities and functionalities remain a formidable challenge in organometallic supramolecular chemistry. Here, we report two half-sandwich iridium-based metallarectangles, [Cp₂Ir₂Cl₂]₂L₂(OTf)₄ (1) and [Cp₂Ir₂(<em>μ</em>-DHBQ)]₂L₂(OTf)₄ (2), which were obtained in high yields via coordination-driven self-assembly of binuclear precursors B1 and B2 employing a 2,1,3-benzothiadiazole (BTD)-based bidentate ligand L. Based on single-crystal XRD analysis, the molecular structures of these complexes adopt tetranuclear rectangular macrocyclic architectures with cavities of distinct dimensions. Subsequent NMR titration studies confirmed that metallarectangle 2 exhibits exceptional host-guest properties, notably encapsulating electron-rich polycyclic aromatic hydrocarbons (PAHs) such as anthracene, phenanthrene, and pyrene. Additionally, the crystal structure of complex 2⊃pyrene provides molecular-level insight into the key interactions governing host-guest assembly and stability.</div></div>","PeriodicalId":374,"journal":{"name":"Journal of Organometallic Chemistry","volume":"1046 ","pages":"Article 123998"},"PeriodicalIF":2.1,"publicationDate":"2025-12-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145882164","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Testing cuprophilicity with tetrahedral ruthenium hydride carbonyl clusters 用四面体氢化钌羰基团簇测试亲铜性
IF 2.1 3区 化学 Q3 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-12-29 DOI: 10.1016/j.jorganchem.2025.123999
Cristiana Cesari , Marco Bortoluzzi , Cristina Femoni , Francesca Forti , Maria Carmela Iapalucci , Giorgia Scorzoni , Stefano Zacchini
The reaction of [NEt4]3 [HRu4(CO)12] (1) with three mole equivalents of [Cu(MeCN)4][BF4] and three mole equivalents of [NEt4]Br affords a nearly 1:1 mixture of [NEt4]3 [HRu4(CO)12(CuBr)3] (2) and [NEt4]2 [H2Ru8(CO)24Cu7Br3] (3). These two products can be separated owing to their different solubilities in organic solvents. [NEt4]3 [HRu8(CO)24Cu6Br2] (4) has been obtained reacting 1, [Cu(MeCN)4][BF4] and [NEt4]Br with stoichiometry 1:1:3. In the absence of [NEt4]Br, 1 reacts with 3.5 mole equivalents of [Cu(MeCN)4][BF4] affording [Ru5(CO)15(CuMeCN)2] (5). The new clusters 25 have been fully characterized by FT-IR and 1H NMR spectroscopy, and their molecular structures elucidated by single-crystal X-ray diffraction (SC-XRD). Homometallic Ru-Ru and Cu-Cu as well as heterometallic Ru-Cu interactions have been computationally investigated by DFT methods.
[NEt4]3 [HRu4(CO)12](1)与3摩尔当量的[Cu(MeCN)4][BF4]和3摩尔当量的[NEt4]Br反应,得到[NEt4]3 [HRu4(CO)12(cur)3](2)和[NEt4]2 [H2Ru8(CO)24Cu7Br3](3)的接近1:1的混合物。这两种产物在有机溶剂中的溶解度不同,因此可以分离。[NEt4]3 [HRu8(CO)24Cu6Br2](4)与[Cu(MeCN)4][BF4]和[NEt4]Br反应,化学计量比为1:1:3。在没有[NEt4]Br的情况下,1与3.5摩尔当量的[Cu(MeCN)4][BF4]反应生成[Ru5(CO)15(CuMeCN)2](5)。利用FT-IR和1H NMR对新簇2-5进行了全面表征,并用单晶x射线衍射(SC-XRD)对其分子结构进行了表征。用离散傅立叶变换方法计算研究了同金属Ru-Ru和Cu-Cu以及异质金属Ru-Cu相互作用。
{"title":"Testing cuprophilicity with tetrahedral ruthenium hydride carbonyl clusters","authors":"Cristiana Cesari ,&nbsp;Marco Bortoluzzi ,&nbsp;Cristina Femoni ,&nbsp;Francesca Forti ,&nbsp;Maria Carmela Iapalucci ,&nbsp;Giorgia Scorzoni ,&nbsp;Stefano Zacchini","doi":"10.1016/j.jorganchem.2025.123999","DOIUrl":"10.1016/j.jorganchem.2025.123999","url":null,"abstract":"<div><div>The reaction of [NEt<sub>4</sub>]<sub>3</sub> [HRu<sub>4</sub>(CO)<sub>12</sub>] (<strong>1</strong>) with three mole equivalents of [Cu(MeCN)<sub>4</sub>][BF<sub>4</sub>] and three mole equivalents of [NEt<sub>4</sub>]Br affords a nearly 1:1 mixture of [NEt<sub>4</sub>]<sub>3</sub> [HRu<sub>4</sub>(CO)<sub>12</sub>(CuBr)<sub>3</sub>] (<strong>2</strong>) and [NEt<sub>4</sub>]<sub>2</sub> [H<sub>2</sub>Ru<sub>8</sub>(CO)<sub>24</sub>Cu<sub>7</sub>Br<sub>3</sub>] (<strong>3</strong>). These two products can be separated owing to their different solubilities in organic solvents. [NEt<sub>4</sub>]<sub>3</sub> [HRu<sub>8</sub>(CO)<sub>24</sub>Cu<sub>6</sub>Br<sub>2</sub>] (<strong>4</strong>) has been obtained reacting <strong>1</strong>, [Cu(MeCN)<sub>4</sub>][BF<sub>4</sub>] and [NEt<sub>4</sub>]Br with stoichiometry 1:1:3. In the absence of [NEt<sub>4</sub>]Br, <strong>1</strong> reacts with 3.5 mole equivalents of [Cu(MeCN)<sub>4</sub>][BF<sub>4</sub>] affording [Ru<sub>5</sub>(CO)<sub>15</sub>(CuMeCN)<sub>2</sub>] (<strong>5</strong>). The new clusters <strong>2</strong>–<strong>5</strong> have been fully characterized by FT-IR and <sup>1</sup>H NMR spectroscopy, and their molecular structures elucidated by single-crystal X-ray diffraction (SC-XRD). Homometallic Ru-Ru and Cu-Cu as well as heterometallic Ru-Cu interactions have been computationally investigated by DFT methods.</div></div>","PeriodicalId":374,"journal":{"name":"Journal of Organometallic Chemistry","volume":"1046 ","pages":"Article 123999"},"PeriodicalIF":2.1,"publicationDate":"2025-12-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145882163","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Design and synthesis of novel phthalazine and benzofuran scaffolds using CoFe₂O₄@CNSCu nanocatalyst: Evaluation of PARP-1 inhibitory activity 用CoFe₂O₄@CNSCu纳米催化剂设计合成新型酞嗪和苯并呋喃支架:PARP-1抑制活性评价
IF 2.1 3区 化学 Q3 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-12-28 DOI: 10.1016/j.jorganchem.2025.123997
Firouz Matloubi Moghaddam, Hassan Fazli, Shaghayegh Sadredini
A magnetically recoverable nanocatalyst, CoFe₂O₄@CNSCu, was prepared via a three-step procedure: (i) co-precipitation synthesis of CoFe₂O₄ nanoparticles, (ii) coating with HKUST-1 through a mercaptoacetic acid linker, and (iii) formation of a carbon–sulfur framework from thioacetamide under nitrogen. The catalyst was fully characterized by XRD, FE-SEM, and TEM. It was applied in a three-component reaction for the synthesis of novel triazole-based hybrids containing either 2-phenyl-2,3-dihydro-phthalazine-1,4‑dione or benzofuran units. Under optimized conditions (5 mol% catalyst, DMSO/H₂O 1:1, room temperature, 1 h), a wide range of products were obtained in good to excellent isolated yields (61–96%) and high purity. The CoFe₂O₄@CNSCu nanocatalyst efficiently generates Cu(I) active species in situ, enabling smooth 1,3-dipolar cycloaddition while allowing easy magnetic separation and reuse. The method tolerated various alkyl halides, including electron-donating, electron-withdrawing, and sterically demanding groups, highlighting its generality and practical applicability. Preliminary biological evaluation revealed that the new hybrids strongly inhibited PARP-1, suggesting their potential as promising leads for anticancer drug development.
采用三步法制备了一种磁性可回收纳米催化剂CoFe₂O₄@CNSCu: (i)共沉淀法合成CoFe₂O₄纳米颗粒;(ii)通过巯基乙酸连接剂涂覆HKUST-1; (iii)硫代乙酰胺在氮气作用下形成碳硫骨架。通过XRD、FE-SEM和TEM对催化剂进行了表征。将其应用于三组分反应中,合成了含有2-苯基-2,3-二氢酞嗪-1,4 -二酮或苯并呋喃的新型三唑基杂化物。在优化条件下(5 mol%催化剂,DMSO/H₂O 1:1,室温,1 H),可获得多种产品,分离率为61 ~ 96%,纯度高。CoFe₂O₄@CNSCu纳米催化剂有效地原位生成Cu(I)活性物质,实现光滑的1,3-偶极环加成,同时易于磁分离和重复使用。该方法可耐受各种烷基卤化物,包括给电子、吸电子和要求立体的基团,突出了其通用性和实用性。初步的生物学评价表明,新的杂交体对PARP-1具有强烈的抑制作用,这表明它们有潜力成为抗癌药物开发的有希望的线索。
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引用次数: 0
Efficient synthesis of substituted 1,4-Dihydropyridines using NiFe-LDH: A green catalytic approach 镍铁- ldh高效合成取代的1,4-二氢吡啶:绿色催化方法
IF 2.1 3区 化学 Q3 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-12-28 DOI: 10.1016/j.jorganchem.2025.123995
Soumaya Talbi , Zhor Ou-ichen , Zineb Tchorbo , Marieme Kacem , Mustapha Dib , Abdelghani Boussetta , Salha Hamri , Souad Rabi , Abderrafia Hafid , Mostafa Khouili
In this work, we describe an eco-friendly approach for the synthesis of 1,4-dihydropyridine (1,4-DHP) derivatives via the reaction of substituted aromatic aldehydes with ethyl acetoacetate and ammonium acetate by using NiFe-LDH solid catalyst. Furthermore, NiFe-LDH catalyst was prepared successfully through a co-precipitation process carried out at pH 10.0 ± 0.2, with a Ni²⁺/Fe³⁺ molar ratio of 3. The synthesized material was extensively analyzed using numerous techniques such as XRD, IR, N2-Adsorption-Desorption and SEM-EDS. The reaction was performed in ethanol as a green solvent, with NiFe-LDH serving as a recyclable heterogeneous catalyst. As result, this methodology provides several benefits, such as mild operating conditions, environmentally sustainable synthesis, high yields reaching 92%, and straightforward catalyst recovery.
在这项工作中,我们描述了一种以NiFe-LDH固体催化剂为催化剂,通过取代芳香醛与乙酰乙酸乙酯和乙酸铵的反应合成1,4-二氢吡啶(1,4- dhp)衍生物的环保方法。在pH 10.0±0.2条件下,Ni 2 + /Fe³+的摩尔比为3,通过共沉淀法成功制备了NiFe-LDH催化剂。采用XRD、IR、n2 -吸附-解吸、SEM-EDS等多种技术对合成材料进行了分析。该反应以乙醇为绿色溶剂,镍铁- ldh作为可回收的多相催化剂进行。因此,该方法具有多种优点,如操作条件温和,合成环境可持续,收率高达92%,催化剂回收率直接。
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引用次数: 0
A green and recyclable salen-cobalt catalyst immobilized on MCM-48 for Pd- and Cu-free sonogashira coupling reaction in aqueous media MCM-48固定化绿色可回收盐钴催化剂用于无钯无铜sonogashira偶联反应
IF 2.1 3区 化学 Q3 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-12-27 DOI: 10.1016/j.jorganchem.2025.123996
Rusul Alabada , Rima Heider Al Omari , Magda H. Abdellattif , G PadmaPriya , Subhashree Ray , Kattela Chennakesavulu , Renu Sharma , Ashish Singh Chauhan
A novel Pd-Cu free heterogeneous catalyst was developed by covalently immobilizing a salen cobalt complex onto the surface of mesoporous silica MCM-48. The mesoporous support provided a high surface area and regular pore arrangement, promoting efficient dispersion and accessibility of active sites. The resulting catalyst was characterized using different techniques including FT-IR, XRD, BET, TEM, SEM, TGA, and ICP-OES to confirm its structural integrity, surface properties, and successful functionalization. The catalyst displayed outstanding performance in the Sonogashira cross-coupling reaction under eco-friendly conditions employing water as a sustainable solvent and in the absence of palladium or copper co-catalysts. A wide range of aryl halides and terminal alkynes were efficiently coupled to obtain the desired products with good to excellent yields. Moreover, the heterogeneous nature of the catalyst allowed for easy recovery and reuse over five cycles with minimal decline in activity or leaching of cobalt. This study presents an effective and sustainable approach to developing non-noble metal catalysts for cross-coupling reactions, highlighting the potential of immobilized Co-salen complexes as versatile and green catalysts in organic transformations.
通过在介孔二氧化硅MCM-48表面共价固定一种新型无钯铜非均相催化剂。介孔支架提供了高的比表面积和规则的孔隙排列,促进了活性位点的有效分散和可达性。利用FT-IR、XRD、BET、TEM、SEM、TGA和ICP-OES等技术对催化剂进行了表征,以确定其结构完整性、表面性能和成功的功能化。该催化剂在环保条件下,以水为可持续溶剂,在无钯或铜共催化剂的情况下,在Sonogashira交叉偶联反应中表现出优异的性能。广泛的芳基卤化物和末端炔被有效地偶联,得到所需的产品,并具有良好的收率。此外,催化剂的非均相性质允许在五个循环中轻松回收和再利用,而活性或钴浸出的下降最小。本研究提出了一种有效和可持续的方法来开发用于交叉偶联反应的非贵金属催化剂,突出了固定化Co-salen配合物作为有机转化中多功能和绿色催化剂的潜力。
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引用次数: 0
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