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Multigram‑scale synthesis of BTK inhibitor BIIB068 BTK抑制剂BIIB068的多图谱合成
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-18 DOI: 10.1007/s11696-023-02951-9
Donghao Jia, Mingfang Gu, Xinyue Yu, Kunyang Yuan, Sixuan Wang, Mingzhang Guo, Ping Gong

This paper describes the development of a relatively feasible, economic, and safe method for the multigram-scale synthesis of BIIB068, an efficient reversible BTK inhibitor. The new process is highlighted by an economical construction of a 2-amino-4 substituted pyrimidine employing a simple nucleophilic substitution reaction and a green reduction of the cyano group. The developed process provided an overall yield of 32%, with an HPLC purity of 99%. The structure of BIIB068 was confirmed by MS, IR, 1H-NMR, and 13C-NMR, and the structures of some intermediates were confirmed by MS and 1H-NMR.

Graphical abstract

本文介绍了一种相对可行、经济、安全的多流程合成高效可逆BTK抑制剂BIIB068的方法。采用简单的亲核取代反应和氰基的绿色还原,经济地构建了2-氨基-4取代的嘧啶,突显了这一新工艺。所开发的方法提供了32%的总产率,HPLC纯度为99%。BIIB068的结构通过MS、IR、1H-NMR和13C-NMR得到了证实,一些中间体的结构也通过MS和1H-NMR得到了证实
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引用次数: 0
Synthesis and electroanalytical applications of a novel hydrazinecarbothioamide derivative molecule 一种新型肼甲硫酰胺衍生物分子的合成及电分析应用
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-17 DOI: 10.1007/s11696-023-02968-0
Oguz Özbek, Serkan Ören, Meliha Burcu Gürdere, Ömer Isildak, Mustafa Ceylan

Molecules containing multiple donor atoms such as nitrogen, oxygen and sulfur in their structure are more preferred as ionophores in the preparation of ion-selective electrodes. In this study, a new hydrazinecarbotioamide derivative molecule was synthesized as an ionophore and characterized using NMR, FT–IR and elemental analysis techniques. The potentiometric electrodes prepared with the synthesized new molecule (ionophore) exhibited selectivity towards lead(II) ions. This novel electrode had a low detection limit of 6.98 × 10–7 M over a wide concentration range of 1.0 × 10–6–1.0 × 10–1 M. Obtained experimental data showed that the electrode has good repeatability, good selectivity and good stability. At the same time, it could work in a wide pH range without being affected by pH changes. The analytical applications of the developed electrode, whose potentiometric performance parameters were studied, were carried out in different water samples.

在离子选择电极的制备中,在其结构中含有多个供体原子如氮、氧和硫的分子更优选作为离子载体。在本研究中,合成了一种新的肼基碳硫酰胺衍生物分子作为离子载体,并用NMR、FT–IR和元素分析技术对其进行了表征。用合成的新分子(离子载体)制备的电位电极对铅(II)离子具有选择性。这种新型电极的检测下限为6.98 × 在1.0的宽浓度范围内为10-7M × 10–6–1.0 × 10-1米。实验数据表明,该电极具有良好的重复性、选择性和稳定性。同时,它可以在宽的pH范围内工作,而不受pH变化的影响。研究了所开发的电极的电位性能参数,并在不同的水样中进行了分析应用。
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引用次数: 1
Sol–gel preparation of spinel ferrites/polyaniline composites for electromagnetic interface shielding 溶胶-凝胶法制备用于电磁界面屏蔽的尖晶石-铁氧体/聚苯胺复合材料
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-15 DOI: 10.1007/s11696-023-02956-4
Muhammad Zeshan, Muhammad Suleman Waheed, Saad Ahmad Ishaq, Abubakar Siddique, Atta Ullah, El-Sayed M. Sherif, Mohd Zahid Ansari, Sajjad Ahmad Khan, Abdul Rauf Khan, Hafiz Muhammad Tahir Farid

In this study, we examined the properties of conductive polymers and related composites that are typically used for EMI shielding owing of their magnetic and microwave properties. Ferrite/polymer (PANI) composites, which have magnetic properties, are a promising area of research for multifunctional materials. Specifically, we compared and contrasted the properties of PANI, gadolinium-substituted spinel ferrite, and their composites. In this research, we employed the sol–gel method to synthesize polyaniline and spinel ferrites. The nanocomposites were formed by combining the polyaniline and spinel ferrites. Various properties of these nanocomposites were analyzed using multiple characterization methods, including X-ray diffraction (XRD), a vibrating sample magnetometer (VSM), Direct current electrical resistivity and microwave. The X-ray diffraction pattern indicated the presence of a pure crystalline ferrite phase, with an average size of the crystallite approximately 40 nm. The ferromagnetic properties of the nanocomposites were demonstrated through the M-H loops. The microwave properties of materials, namely their capacity to reflect or deflect electromagnetic radiation in the appropriate frequency range, impact the effectiveness of EMI shielding for microwave applications.

在这项研究中,我们考察了导电聚合物和相关复合材料的性能,这些材料由于其磁性和微波特性而通常用于EMI屏蔽。铁氧体/聚合物(PANI)复合材料具有良好的磁性,是一个很有前途的多功能材料研究领域。具体而言,我们比较和对比了PANI、钆取代尖晶石铁氧体及其复合材料的性能。在本研究中,我们采用溶胶-凝胶法合成了聚苯胺和尖晶石铁氧体。将聚苯胺和尖晶石型铁氧体结合形成纳米复合材料。使用多种表征方法,包括X射线衍射(XRD)、振动样品磁强计(VSM)、直流电阻率和微波,分析了这些纳米复合材料的各种性能。X射线衍射图表明存在纯结晶铁氧体相,微晶的平均尺寸约为40nm。通过M-H环证明了纳米复合材料的铁磁性能。材料的微波特性,即其在适当频率范围内反射或偏转电磁辐射的能力,影响微波应用中EMI屏蔽的有效性。
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引用次数: 2
Cadmium determination at trace levels in lake water samples by cold vapor generation-atomic absorption spectrometry after magnetic dispersive solid phase extraction 磁分散固相萃取-冷蒸气发生-原子吸收光谱法测定湖水中痕量镉
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-14 DOI: 10.1007/s11696-023-02963-5
Süleyman Bodur, Sezin Erarpat, İnci Kayın, Sezgin Bakırdere

This study established an analytical method based on manganese ferrite based magnetic dispersive solid phase extraction (MDSPE) before cold vapor generation–atomic absorption spectrometry (CVG-AAS) for the determination of cadmium at trace levels in lake water samples collected from Horseshoe Island, Antarctica. Manganese ferrite nanoparticles were synthesized to be used as an adsorbent in the MDSPE method. Different MDSPE and CVG parameters were fixed to their optimum values after univariate optimization approach. Under the optimum conditions, analytical performance of the developed MDSPE-CVG-AAS method was evaluated and its applicability/accuracy was determined by recovery experiments. Twelve different lake water samples collected from Horseshoe Island, Antarctica were analyzed. Matrix matching calibration strategy was used to eliminate possible matrix effects arising from the lake water samples. Good recovery results (93.2–112.5%) were obtained from the spiked samples that indicated the method suitability to real samples.

本研究建立了一种基于锰铁氧体基磁分散固相萃取(MDSPE)的冷蒸汽发生-原子吸收光谱法(CVG-AAS)分析方法,用于测定从南极洲马蹄岛采集的湖水样品中痕量镉。合成了锰铁氧体纳米颗粒,用作MDSPE方法中的吸附剂。在单变量优化方法后,将不同的MDSPE和CVG参数固定到其最佳值。在最佳条件下,对所开发的MDSPE-CVG-AAS方法的分析性能进行了评价,并通过回收实验确定了其适用性/准确性。对从南极洲马蹄岛采集的12个不同的湖水样本进行了分析。使用矩阵匹配校准策略来消除湖水样本可能产生的矩阵效应。从加标样品中获得了良好的回收率结果(93.2–112.5%),表明该方法适用于真实样品。
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引用次数: 0
Microfluidics-facilitated spontaneous synthesis of ZIF-67 metal–organic framework 微流体促进了ZIF-67金属有机骨架的自发合成
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-11 DOI: 10.1007/s11696-023-02944-8
Svapnil Kevat, V. N. Lad
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引用次数: 0
Green synthesis of zinc oxide nanoparticles from Rhododendron arboreum extract and their potential applications in photocatalytic degradation of cationic dyes malachite green and Fuchsin basic dye 树木杜鹃提取物绿色合成氧化锌纳米颗粒及其在光催化降解阳离子染料孔雀石绿和紫红色碱性染料中的潜在应用
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-11 DOI: 10.1007/s11696-023-02960-8
Tanuj, Rajesh Kumar, Santosh Kumar, Neerja Kalra, Subhash Sharma, Amritpal Singh

Hereby, in this paper, we have reported synthesis of uniform spherical-shaped nanoparticles of zinc oxide via green method, as well as their photocatalytic activity. The nanoparticles of zinc oxide were synthesized utilizing flower extract of Rhododendron arboreum where it performs the function of reducing as well as capping agent. The synthesized nanoparticles were characterized by numerous spectroscopic techniques such as UV–Vis and FT-IR. Scanning electron microscope analysis of product revealed spherical zinc oxide nanoparticles. Energy-dispersive spectral analysis indicated elemental composition, i.e., oxygen and zinc. The green synthesized zinc oxide nanoparticles have been employed as nanocatalyst for photocatalytic degradation of two cationic dyes, i.e., Fuchsin basic and Malachite green dye. In addition, various physicochemical parameters such as effect of the dye concentration, catalyst dosage and pH have also been optimized indicating better performance of these nanoparticles. Zinc oxide nanoparticles showed 99.18% degradation of Malachite green dye and 99.272% degradation of Fuchsin basic dye. These nanoparticles have great potential candidate as developing catalyst for selective degradation of cationic dyes.

因此,在本文中,我们报道了通过绿色方法合成均匀球形氧化锌纳米颗粒及其光催化活性。利用杜鹃花提取物合成了氧化锌纳米颗粒,氧化锌具有还原和封端作用。通过紫外-可见光谱和红外光谱等多种光谱技术对合成的纳米颗粒进行了表征。产品的扫描电子显微镜分析显示球形氧化锌纳米颗粒。能量色散光谱分析表明元素组成,即氧和锌。绿色合成的氧化锌纳米颗粒已被用作光催化降解两种阳离子染料的纳米催化剂,即Fucsin碱性染料和孔雀石绿染料。此外,还优化了各种物理化学参数,如染料浓度、催化剂用量和pH的影响,表明这些纳米颗粒具有更好的性能。氧化锌纳米粒子对孔雀绿染料的降解率为99.18%,对富铬碱性染料的降解度为99.272%。这些纳米颗粒作为阳离子染料选择性降解的发展催化剂具有很大的潜力。
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引用次数: 2
Studying loading of 5-fluorouracil onto the surface of gold–silver nanocomposite utilizing DLS and UV–Vis spectroscopy 利用DLS和紫外可见光谱研究5-氟尿嘧啶在金银纳米复合材料表面的负载
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-10 DOI: 10.1007/s11696-023-02927-9
Zhengqiao Liu, Zeran Yu, Lingfeng Zhang, Reza Tayebee, Shohre Pourmojahed, Effat Esmaeili Shahri, Xu Chen
<div><p>The antimetabolite drug 5-fluorouracil (5-Fu) is extensively applied to treat many cancerous tumors. However, in order to inhibit its severe side effects and maintain its clinical benefits and anticancer efficacy, this drug should be loaded onto a suitable nanovehicle. In this work, gold nanoparticles were synthesized using Turkevich reduction method, and then, the prepared particles coated with a thin layer of silver via re-reduction of a silver nitrate solution. XRD, EDS, DLS, TEM and UV–Visible measurements were performed to characterize gold and gold–silver nanoparticles. By taking the UV–Visible absorption spectrum, two plasmonic peaks found at 411 and 526 nm due to the localized surface plasmons of the spherical interfaces of the nanoparticles. By loading 5-fluorouracil molecules onto the surface of gold and fabrication of gold–silver nanocomposite, significant changes occurred in the TEM, DLS and UV–Vis outcomes that can be interpreted considering the re-decoration and aggregation of the nanoparticles. Moreover, both of the plasmonic peaks experienced a redshift. By adding different amounts of drug solution into the colloidal solution, a direct and meaningful relation was obtained between the absorption peaks and drug concentration, which can be used as a measuring tool to evaluate drug loading amount. This study revealed that 5-fluorouracil affects DLS and UV–Vis absorption characteristics of gold–silver nanocomposite and adsorption characteristics of the synthesized bimetallic Ag–Au nanocomposite leading to more suitable results compared to the single metal nanoparticles. It is concluded that measuring drug loading using gold–silver nanocomposite would be more precise than that of single metal nanoparticles. In addition, the drug release behavior of drug-loaded gold–silver nanocomposite was also investigated under in vitro conditions at pH 6.5 and 37 °C. This study revealed that ~ 72% of loaded drug was released after 70 h. Furthermore, the MTT assay was used to study the cytocompatibility of the loaded drug on the cancer cell line U251. This study showed that the drug-loaded nanoparticles have a higher anti-proliferative effect compared to that of the free drug against U251 glioma cancer cells.</p><h3>Graphical abstract</h3><p>5-Fluorouracil as an extensively used drug in the treatment of many cancers is delivered by gold–silver nanocomposite. Findings revealed that the bimetallic nanocomposite behaves much better than the corresponding single metal counterparts in the drug loading process. Loading of 5-fluorouracil molecules onto the surface of gold–silver nanoparticles significantly affects TEM, DLS and optical properties of the carrier, and therefore, a direct and meaningful relation can be obtained between the peak changes and drug concentration. In addition, the prepared nanoparticles showed acceptable anti-proliferative activity against the cancer cell line U251.</p> <figure><div><div><div><picture><sourc
抗代谢药物5-氟尿嘧啶(5-Fu)广泛应用于治疗多种恶性肿瘤。然而,为了抑制其严重的副作用,保持其临床疗效和抗癌效果,必须将其装载到合适的纳米载体上。本研究采用Turkevich还原法制备金纳米颗粒,并通过硝酸银溶液的再还原法制备了一层薄银。采用XRD、EDS、DLS、TEM和uv -可见等方法对金、金银纳米颗粒进行表征。通过紫外可见吸收光谱,在411 nm和526 nm处发现了两个等离子体峰,这是由于纳米颗粒球面界面的局部表面等离子体引起的。通过将5-氟尿嘧啶分子加载到金表面并制备金-银纳米复合材料,TEM、DLS和UV-Vis结果发生了显著变化,这可以解释为纳米颗粒的重新装饰和聚集。此外,两个等离子体峰都经历了红移。通过在胶体溶液中加入不同量的药物溶液,获得了吸收峰与药物浓度之间的直接关系,可作为评价载药量的测量工具。本研究发现,5-氟尿嘧啶影响了金银纳米复合材料的DLS和UV-Vis吸收特性,以及合成的Ag-Au双金属纳米复合材料的吸附特性,导致比单金属纳米颗粒更合适的结果。结果表明,利用金银纳米复合材料测量药物负载比单金属纳米颗粒测量更精确。此外,还考察了载药金银纳米复合材料在pH 6.5和37℃条件下的体外释药行为。结果表明,载药70 h后释药量约为72%。此外,利用MTT法研究了载药在U251癌细胞上的细胞相容性。本研究表明,与游离药物相比,载药纳米颗粒对U251胶质瘤细胞具有更高的抗增殖作用。图形摘要5-氟尿嘧啶是一种广泛应用于多种癌症治疗的药物,它是由金银纳米复合材料输送的。结果表明,双金属纳米复合材料在载药过程中的表现明显优于相应的单金属纳米复合材料。负载5-氟尿嘧啶分子到金-银纳米颗粒表面对载体的TEM、DLS和光学性能有显著影响,因此峰变化与药物浓度之间有直接而有意义的关系。此外,制备的纳米颗粒对癌细胞U251具有良好的抗增殖活性。
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引用次数: 1
A mathematical investigation into the limited use of energy recovery devices in brackish water reverse osmosis processes 对微咸水反渗透过程中有限使用能量回收装置的数学研究
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-09 DOI: 10.1007/s11696-023-02949-3
Bhaumik Sutariya
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引用次数: 0
Synthesis and characterization of Cu/EMC-2 zeolite by two routes 两种途径合成Cu/EMC-2沸石及表征
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-07 DOI: 10.1007/s11696-023-02947-5
A. Medina-Ramirez, Francisco J. Morado-Alcantar, I. Galindo-Esquivel, J. Díaz-Guillén, C. M. Lopez Badillo
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引用次数: 0
Bithiophene-naphthalene chalcone as a fluorescent pigment in eco-friendly security ink formulation 二噻吩-萘-查尔酮作为环保安全油墨配方中的荧光颜料
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-07 DOI: 10.1007/s11696-023-02958-2
Rakshitha K. Jain, Kashmitha Muthamma, Dhanya Sunil, Suresh D. Kulkarni, P. J. Anand, Nilanjan Dey

Approaches to prevent document/product forgery using eco-friendly printing inks and security printing techniques on flexible substrates are two vital areas of research that demand coherent advancements. In this context, a new bithiophene-naphthalene chalcone (BTNP) was synthesized and characterized as a fluorescent pigment for use in security ink. BTNP exhibited good solid-state and solution phase fluorescence with intramolecular charge transfer confirmed using theoretical studies and emission spectra collected in THF/THF–hexane mixtures. The aggregation-induced emission of BTNP was established using solution phase studies in THF/THF–water mixtures. The strong solid-state yellow emission of BTNP prompted its use as a pigment in the preparation of an environment-friendly UV fluorescent formulation, devoid of any volatile organic compounds or hazardous air pollutants. The screen prints obtained on a UV dull paper substrate utilizing BTNP ink revealed good fluorescence, photostability, colorimetric, densitometric, and rub resistance characteristics, which showcase the potential applicability of the BTNP formulation in security printing. The low cytotoxic nature of the chalcone as observed in the MTT assay could also be exploited for the use of formulation in inkpads.

Graphical abstract

使用环保印刷油墨防止文件/产品伪造的方法和在柔性基底上的安全印刷技术是两个需要连贯进步的重要研究领域。在此背景下,合成了一种新的双噻吩萘查尔酮(BTNP),并将其表征为用于安全油墨的荧光颜料。BTNP表现出良好的固态和溶液相荧光,分子内电荷转移通过理论研究和在THF/THF–己烷混合物中收集的发射光谱得到证实。BTNP的聚集诱导发射是通过在THF/THF-水混合物中的溶液相研究确定的。BTNP强烈的固态黄色发射促使其作为颜料用于制备环境友好的紫外线荧光制剂,不含任何挥发性有机化合物或有害空气污染物。使用BTNP油墨在UV暗纸基材上获得的丝网印刷显示出良好的荧光、光稳定性、色度、密度计和耐摩擦特性,这展示了BTNP配方在安全印刷中的潜在适用性。在MTT测定中观察到的查尔酮的低细胞毒性性质也可用于在墨垫中使用制剂。图形摘要
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引用次数: 0
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