Pub Date : 2024-05-28DOI: 10.1007/s00706-024-03219-y
Huda Abdalkarem M. Sadeq Alı Yashıl, İrem Okman Koçoğlu
In this study, an amperometric dopamine sensor based on carbon nanofibers (CNF), Fe3O4 nanoparticles (Fe3O4NP), and silver nanoparticles (AgNP) modified glassy carbon electrode (GCE) was developed. In order to determine the optimum surface composition, the effects of CNF amount, Fe3O4 amount and the electrodeposition step of AgNP were investigated. Optimum experimental parameters such as working potential and pH of test solution were also explored. The morphological and electrochemical properties of the AgNP/CNF − Fe3O4NP/GCE were studied using scanning electron microscopy, cyclic voltammetry, and chronoamperometry. The AgNP/CNF − Fe3O4NP/GCE showed linear response to dopamine between 2.0 × 10−7 and 5.5 × 10−4 M with a detection limit of 1.8 × 10−7 M and sensitivity of 37.24 μA mM−1. Analytical performance characteristics such as reproducibility, reusability, and selectivity were also investigated for the presented dopamine sensor. The sensor was successfully applied to the detection of dopamine in dopamine hydrochloride injection samples using the standard addition method and good recoveries were obtained.
{"title":"Amperometric dopamine sensor based on carbon nanofiber, Fe3O4 nanoparticles, and silver nanoparticles modified glassy carbon electrode","authors":"Huda Abdalkarem M. Sadeq Alı Yashıl, İrem Okman Koçoğlu","doi":"10.1007/s00706-024-03219-y","DOIUrl":"https://doi.org/10.1007/s00706-024-03219-y","url":null,"abstract":"<p>In this study, an amperometric dopamine sensor based on carbon nanofibers (CNF), Fe<sub>3</sub>O<sub>4</sub> nanoparticles (Fe<sub>3</sub>O<sub>4</sub>NP), and silver nanoparticles (AgNP) modified glassy carbon electrode (GCE) was developed. In order to determine the optimum surface composition, the effects of CNF amount, Fe<sub>3</sub>O<sub>4</sub> amount and the electrodeposition step of AgNP were investigated. Optimum experimental parameters such as working potential and pH of test solution were also explored. The morphological and electrochemical properties of the AgNP/CNF − Fe<sub>3</sub>O<sub>4</sub>NP/GCE were studied using scanning electron microscopy, cyclic voltammetry, and chronoamperometry. The AgNP/CNF − Fe<sub>3</sub>O<sub>4</sub>NP/GCE showed linear response to dopamine between 2.0 × 10<sup>−7</sup> and 5.5 × 10<sup>−4</sup> M with a detection limit of 1.8 × 10<sup>−7</sup> M and sensitivity of 37.24 μA mM<sup>−1</sup>. Analytical performance characteristics such as reproducibility, reusability, and selectivity were also investigated for the presented dopamine sensor. The sensor was successfully applied to the detection of dopamine in dopamine hydrochloride injection samples using the standard addition method and good recoveries were obtained.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"62 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141165475","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Two polyamine-diarylidenyl piperidone (DAP) derivatives, dimer polyamine-H-4073 and tetrameric polyamine-H-4073, were designed and synthesized as antitumor agents by coupling the bifluoro-substituted DAP STAT3 inhibitor H-4073 to two different polyamines through the binary fatty acid chains, respectively. MTT assay and a SW480 xenograft model identified dimer polyamine-H-4073 as good candidate antitumor agent with good efficacy, limited toxicity, and low resistance, in comparison with H-4073, cisplatin, and doxorubicin. Western blot analysis results indicated that dimer polyamine-H-4073 exhibited effectively inhibition on signal transducer and activator of transcription 3 (STAT3), indicating that it may be a STAT3 inhibitor.
{"title":"Synthesis and pharmacological evaluation of polyamine-diarylidenyl piperidone derivatives as potent antitumor agents","authors":"Zhi-Chen Mao, Shuang-Qiang Liu, Xiao-Man Chen, Jian-Hua Wei, Ri-Zhen Huang, Ye Zhang","doi":"10.1007/s00706-024-03220-5","DOIUrl":"https://doi.org/10.1007/s00706-024-03220-5","url":null,"abstract":"<p>Two polyamine-diarylidenyl piperidone (DAP) derivatives, dimer polyamine-H-4073 and tetrameric polyamine-H-4073, were designed and synthesized as antitumor agents by coupling the bifluoro-substituted DAP STAT3 inhibitor H-4073 to two different polyamines through the binary fatty acid chains, respectively. MTT assay and a SW480 xenograft model identified dimer polyamine-H-4073 as good candidate antitumor agent with good efficacy, limited toxicity, and low resistance, in comparison with H-4073, cisplatin, and doxorubicin. Western blot analysis results indicated that dimer polyamine-H-4073 exhibited effectively inhibition on signal transducer and activator of transcription 3 (STAT3), indicating that it may be a STAT3 inhibitor.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"34 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141151533","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A starch-supported cuprous iodide nanoparticles (CuI-NPs@starch) catalysed C–C bond cleaving reaction involving carbon-based leaving groups like malononitrile, ethyl cyanoacetate, acetylacetone, and Meldrum’s acid has been developed under moisture and air insensitive conditions. This competent C–C bond cleavage reaction is studied in detail as an attractive alternative method to synthesize biologically relevant bisindolylmethanes in moderate to good yields. The CuI-NPs@starch are synthesized in aqueous medium and characterized by X-ray powder diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy studies.
Graphical abstract
在对湿度和空气不敏感的条件下，开发了一种淀粉支撑的碘化亚铜纳米粒子（CuI-NPs@淀粉）催化的 C-C 键裂解反应，该反应涉及丙二腈、氰乙酸乙酯、乙酰丙酮和梅尔德鲁姆酸等碳基离去基团。我们详细研究了这种有效的 C-C 键裂解反应，将其作为一种有吸引力的替代方法，以中等至较高的产率合成与生物相关的双吲哚甲烷。CuI-NPs@starch 是在水介质中合成的，并通过 X 射线粉末衍射、扫描电子显微镜、能量色散 X 射线光谱研究对其进行了表征。
{"title":"Starch-supported cuprous iodide nanoparticles catalysed C–C bond cleavage: use of carbon-based leaving groups for bisindolylmethane synthesis","authors":"Muthiah Suresh, Raj Bahadur Singh, Sadhana Katlakunta, Snigdha Rani Patra, Yogesh Bhaskar Singh Tanwer, Sadhucharan Mallick, Sabyasachi Bhunia, Debjit Das","doi":"10.1007/s00706-024-03215-2","DOIUrl":"https://doi.org/10.1007/s00706-024-03215-2","url":null,"abstract":"<p>A starch-supported cuprous iodide nanoparticles (CuI-NPs@starch) catalysed C–C bond cleaving reaction involving carbon-based leaving groups like malononitrile, ethyl cyanoacetate, acetylacetone, and Meldrum’s acid has been developed under moisture and air insensitive conditions. This competent C–C bond cleavage reaction is studied in detail as an attractive alternative method to synthesize biologically relevant bisindolylmethanes in moderate to good yields. The CuI-NPs@starch are synthesized in aqueous medium and characterized by X-ray powder diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy studies.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"29 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141061967","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-09DOI: 10.1007/s00706-024-03201-8
Akram Ashouri, Somayeh Pourian, Behzad Nasiri
Phosphine@Pd@Fe3O4 nanomagnetic particles were synthesized through in situ or direct immobilization of the phosphine ligand on metal-coated Fe3O4. These separable heterogeneous nanoparticles were employed as highly efficient catalysts for the arylation of aldehydes using boron reagents, yielding up to 90% within 30 min. The synthesized catalysts were easily recovered through simple magnetic decantation and exhibited no significant decrease in activity upon reuse. The structure and morphology of the nanomagnetic particles were characterized using various techniques, including energy-dispersive X-ray spectroscopy, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis, differential thermal analysis, X-ray diffraction, vibrating-sample magnetometer analysis, and FT-IR spectroscopy.
Graphical abstract
通过在金属包覆的 Fe3O4 上原位或直接固定膦配体，合成了膦@Pd@Fe3O4 纳米磁性粒子。这些可分离的异质纳米粒子被用作高效催化剂，用于使用硼试剂进行醛的芳基化反应，30 分钟内的产率高达 90%。合成的催化剂通过简单的磁性倾析即可轻松回收，重复使用后活性没有明显下降。利用能量色散 X 射线光谱、扫描电子显微镜、透射电子显微镜、热重分析、差热分析、X 射线衍射、振动样品磁力计分析和傅立叶变换红外光谱等多种技术对纳米磁性颗粒的结构和形态进行了表征。
{"title":"Phosphine-coated Pd@Fe3O4 nanoparticles: a highly efficient and magnetically recyclable nanocatalyst for the arylation of aldehyde","authors":"Akram Ashouri, Somayeh Pourian, Behzad Nasiri","doi":"10.1007/s00706-024-03201-8","DOIUrl":"https://doi.org/10.1007/s00706-024-03201-8","url":null,"abstract":"<p>Phosphine@Pd@Fe<sub>3</sub>O<sub>4</sub> nanomagnetic particles were synthesized through in situ or direct immobilization of the phosphine ligand on metal-coated Fe<sub>3</sub>O<sub>4</sub>. These separable heterogeneous nanoparticles were employed as highly efficient catalysts for the arylation of aldehydes using boron reagents, yielding up to 90% within 30 min. The synthesized catalysts were easily recovered through simple magnetic decantation and exhibited no significant decrease in activity upon reuse. The structure and morphology of the nanomagnetic particles were characterized using various techniques, including energy-dispersive X-ray spectroscopy, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis, differential thermal analysis, X-ray diffraction, vibrating-sample magnetometer analysis, and FT-IR spectroscopy.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"8 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140930837","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Eight new bisbenzimidazolium halides were prepared from alkyl halides and 4,4′-bis[(benzimidazol-1-yl)methyl]-1,1′-biphenyl.The structures of the benzimidazole salts were characterized using elemental analysis techniques as well as 1H, 13C NMR, and FT-IR spectroscopic methods. The inhibitory effects of the benzimidazole derivatives were measured against human carbonic anhydrase I (hCA I), human carbonic anhydrase II (hCA II), and acetylcholinesterase (AChE) enzymes. All benzimidazolium halides exhibited significant enzyme inhibitory properties. They showed highly potent inhibitory effect on AChE and hCAs (Ki values are in the range of 15.7 ± 0.8 to 49.7 ± 10.1 nM, 14.6 ± 1.5 to 70.7 ± 2.7 nM, and 17.4 ± 2.8 to 38 ± 10 nM for AChE, hCA I, and hCA II, respectively). The binding orientation of the synthesized bisbenzimidazolium halides was evaluated by molecular docking studies, reflecting the importance of the p-methylbenzyl, m-methylbenzyl, p-nitrophenethyl, and 3-(1,3-dioxoisoindolin-2-yl)methyl) groups in protein–ligand interaction. The docking results support the Ki values of the respective compounds in this study. The structure–activity relationships against the various targets are clearly shown in three dimensions at the atomic level by their interactions with the mentioned enzymes.
{"title":"Bisbenzimidazole salts and their in silico–in vitro inhibitory abilities on hCA I, hCA II, and AChE enzymes","authors":"Ülkü Yılmaz, Yeliz Demir, Tuğba Taşkın Tok, Yetkin Gök, Aydın Aktaş, İlhami Gülçin","doi":"10.1007/s00706-024-03204-5","DOIUrl":"https://doi.org/10.1007/s00706-024-03204-5","url":null,"abstract":"<p>Eight new bisbenzimidazolium halides were prepared from alkyl halides and 4,4′-bis[(benzimidazol-1-yl)methyl]-1,1′-biphenyl.The structures of the benzimidazole salts were characterized using elemental analysis techniques as well as <sup>1</sup>H, <sup>13</sup>C NMR, and FT-IR spectroscopic methods. The inhibitory effects of the benzimidazole derivatives were measured against human carbonic anhydrase I (hCA I), human carbonic anhydrase II (hCA II), and acetylcholinesterase (AChE) enzymes. All benzimidazolium halides exhibited significant enzyme inhibitory properties. They showed highly potent inhibitory effect on AChE and hCAs (<i>K</i><sub><i>i</i></sub> values are in the range of 15.7 ± 0.8 to 49.7 ± 10.1 nM, 14.6 ± 1.5 to 70.7 ± 2.7 nM, and 17.4 ± 2.8 to 38 ± 10 nM for AChE, hCA I, and hCA II, respectively). The binding orientation of the synthesized bisbenzimidazolium halides was evaluated by molecular docking studies, reflecting the importance of the <i>p</i>-methylbenzyl, <i>m</i>-methylbenzyl, <i>p</i>-nitrophenethyl, and 3-(1,3-dioxoisoindolin-2-yl)methyl) groups in protein–ligand interaction. The docking results support the <i>K</i><sub><i>i</i></sub> values of the respective compounds in this study. The structure–activity relationships against the various targets are clearly shown in three dimensions at the atomic level by their interactions with the mentioned enzymes.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"22 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140930756","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-08DOI: 10.1007/s00706-024-03216-1
Matthias R. Steiner, Christoph Marschner, Judith Baumgartner, Johann A. Hlina, Christian Slugovc
Phosphonium phenolate zwitterions have been synthesized from 2,4-di-tert-butyl-6-(diphenylphosphino)phenol and five different oxirane derivatives. The reaction does not proceed at a detectable rate when the two reactants are combined in dichloromethane at room temperature. Despite the substantial ring strain, the reaction proceeds only with the addition of methanol, which acts as a hydrogen transfer shuttle, allowing a slow conversion to the desired zwitterions. The compounds have been fully characterized and single crystal X-ray crystallography has been performed on the methyloxirane and the phenyl glycidyl ether-derived zwitterion. The phosphonium phenolate units exhibit an ylidic bonding situation as evidenced by spectroscopic and crystallographic analysis. Glycidyl ethers were found to react faster than alkyl and aryloxiranes. Decomposition studies of the zwitterions showed high thermal stability in solution under ambient conditions. Under forced conditions (150 °C, 6 h), decomposition to the corresponding phosphine oxide and secondary aliphatic alcohols, the formally hydrogenated oxirane derivative, was observed.
Graphical abstract
我们用 2,4- 二叔丁基-6-（二苯基膦）苯酚和五种不同的环氧乙烷衍生物合成了膦苯酚齐聚物。室温下，当两种反应物在二氯甲烷中结合时，反应不会以可检测到的速率进行。尽管存在很大的环应变，但只有在加入甲醇后反应才会进行，甲醇起着氢传递穿梭器的作用，使反应缓慢地转化为所需的齐聚物。对这些化合物进行了全面的表征，并对甲基环氧乙烷和苯基缩水甘油醚衍生的齐聚物进行了单晶 X 射线晶体学研究。光谱和晶体学分析表明，膦苯酚单元显示出一种酰键情况。研究发现缩水甘油醚的反应速度比烷基和芳基环氧乙烷快。对这些齐聚物的分解研究表明，在环境条件下，它们在溶液中具有很高的热稳定性。在强制条件下（150 °C，6 小时），观察到分解为相应的氧化膦和仲脂肪醇，即正式氢化的环氧乙烷衍生物。
{"title":"Synthesis, characterization and stability of phosphonium phenolate zwitterions derived from a (diphenylphosphino)phenol derivative and oxiranes","authors":"Matthias R. Steiner, Christoph Marschner, Judith Baumgartner, Johann A. Hlina, Christian Slugovc","doi":"10.1007/s00706-024-03216-1","DOIUrl":"https://doi.org/10.1007/s00706-024-03216-1","url":null,"abstract":"<p>Phosphonium phenolate zwitterions have been synthesized from 2,4-di-<i>tert</i>-butyl-6-(diphenylphosphino)phenol and five different oxirane derivatives. The reaction does not proceed at a detectable rate when the two reactants are combined in dichloromethane at room temperature. Despite the substantial ring strain, the reaction proceeds only with the addition of methanol, which acts as a hydrogen transfer shuttle, allowing a slow conversion to the desired zwitterions. The compounds have been fully characterized and single crystal X-ray crystallography has been performed on the methyloxirane and the phenyl glycidyl ether-derived zwitterion. The phosphonium phenolate units exhibit an ylidic bonding situation as evidenced by spectroscopic and crystallographic analysis. Glycidyl ethers were found to react faster than alkyl and aryloxiranes. Decomposition studies of the zwitterions showed high thermal stability in solution under ambient conditions. Under forced conditions (150 °C, 6 h), decomposition to the corresponding phosphine oxide and secondary aliphatic alcohols, the formally hydrogenated oxirane derivative, was observed.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"2015 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140930940","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
[3 + 2] Cycloaddition reaction of N-methyltrifluoromethylmethylene nitrone (MFN) and 2E,4E-5-(benzo[1,3]dioxol-5-yl)-1-(piperidin-1-yl)penta-2,4-dien-1-one (BPD) is studied using molecular electron density theory. The Parr functions analysis predicted successfully the local reactivities and consequent regioselectivity. The calculation of the reaction and activation Gibbs free energies confirmed that the formation of the reported major product under the experimental conditions is more favorable both kinetically and thermodynamically. The origin of this diastereoselectivity was explained by employing IGMH analysis. ELF analysis suggests that the reaction proceeds via a two-stage one-step mechanism and single bonds are formed via coupling of the pseudoradical centers and polarization of the non-bonding electrons.
{"title":"A molecular electron density theory study on the [3 + 2] cycloaddition reaction of a 2,4-dienone and a nitrone: regioselectivity, diastereoselectivity, energetic aspects, and molecular mechanism","authors":"Mousa Soleymani, Mahdieh Chegeni, Negin Daei, Reza Khazaeinejad","doi":"10.1007/s00706-024-03208-1","DOIUrl":"https://doi.org/10.1007/s00706-024-03208-1","url":null,"abstract":"<p>[3 + 2] Cycloaddition reaction of <i>N</i>-methyltrifluoromethylmethylene nitrone (<b>MFN</b>) and 2<i>E</i>,4<i>E</i>-5-(benzo[1,3]dioxol-5-yl)-1-(piperidin-1-yl)penta-2,4-dien-1-one (<b>BPD</b>) is studied using molecular electron density theory. The Parr functions analysis predicted successfully the local reactivities and consequent regioselectivity. The calculation of the reaction and activation Gibbs free energies confirmed that the formation of the reported major product under the experimental conditions is more favorable both kinetically and thermodynamically. The origin of this diastereoselectivity was explained by employing IGMH analysis. ELF analysis suggests that the reaction proceeds via a two-stage one-step mechanism and single bonds are formed via coupling of the pseudoradical centers and polarization of the non-bonding electrons.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"15 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140941914","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-07DOI: 10.1007/s00706-024-03213-4
Vadim V. Bardin, Nicolay Yu. Adonin
A series of acids ArB(OH)2 and Ar2BOH with an electron-withdrawing aryl group were obtained from the corresponding borates K[ArBF3] and K[Ar2BF2] by the action of MX3 (M = B, Al; X = Cl, Br) and subsequent hydrolysis.
{"title":"Preparation of arylboronic and diarylborinic acids from potassium aryl(fluoro)borates","authors":"Vadim V. Bardin, Nicolay Yu. Adonin","doi":"10.1007/s00706-024-03213-4","DOIUrl":"https://doi.org/10.1007/s00706-024-03213-4","url":null,"abstract":"<p>A series of acids ArB(OH)<sub>2</sub> and Ar<sub>2</sub>BOH with an electron-withdrawing aryl group were obtained from the corresponding borates K[ArBF<sub>3</sub>] and K[Ar<sub>2</sub>BF<sub>2</sub>] by the action of MX<sub>3</sub> (M = B, Al; X = Cl, Br) and subsequent hydrolysis.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"77 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140941959","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Lead–acid batteries are widely used in medium and large energy storage systems, but their application in emerging technologies has been limited by shortcomings in practical applications, such as low specific capacity and irreversible sulfation. We tried to apply “water-in-salt” electrolytes to novel symmetric lead-based batteries, exploring a variety of active material substrates to show that graphite foil current collector batteries perform best. An elevated concentration of water-in-salt electrolyte can broaden the electrochemical stability window, which enables these batteries to show excellent discharge performance, with a reversible specific capacity of 167 mAh g−1 at a discharge current density of 0.1 A g−1, increasing the active material utilization to 69.6% of theoretical capacity. In addition, the batteries maintained a discharge capacity of 152 mAh g−1 after 800 cycles, with a capacity retention rate of 91%, which is better than most pre-reported values. The charging and discharging mechanisms of the positive electrode were analyzed using Raman, X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, and transmission electron microscopy.
Graphical abstract
铅酸电池被广泛应用于大中型储能系统，但由于其在实际应用中存在比容量低、硫化不可逆等缺点，其在新兴技术中的应用一直受到限制。我们尝试将 "盐包水 "电解质应用于新型对称铅基电池，并探索了多种活性材料基底，结果表明石墨箔集流电池的性能最佳。高浓度的盐中水电解质可拓宽电化学稳定性窗口，从而使这些电池表现出卓越的放电性能，在放电电流密度为 0.1 A g-1 时，可逆比容量为 167 mAh g-1，活性材料利用率提高到理论容量的 69.6%。此外，电池在 800 次循环后仍能保持 152 mAh g-1 的放电容量，容量保持率高达 91%，优于大多数预先报告的数值。利用拉曼光谱、X 射线衍射、X 射线光电子能谱、扫描电子显微镜和透射电子显微镜分析了正极的充电和放电机制。
{"title":"A new symmetrical lead-based battery using a “water-in-salt” electrolyte","authors":"Xinping Duan, Mingqiang Li, Lixiang Wang, Jingwen Li, Shuailiang Xu, Haochen Weng","doi":"10.1007/s00706-024-03205-4","DOIUrl":"https://doi.org/10.1007/s00706-024-03205-4","url":null,"abstract":"<p>Lead–acid batteries are widely used in medium and large energy storage systems, but their application in emerging technologies has been limited by shortcomings in practical applications, such as low specific capacity and irreversible sulfation. We tried to apply “water-in-salt” electrolytes to novel symmetric lead-based batteries, exploring a variety of active material substrates to show that graphite foil current collector batteries perform best. An elevated concentration of water-in-salt electrolyte can broaden the electrochemical stability window, which enables these batteries to show excellent discharge performance, with a reversible specific capacity of 167 mAh g<sup>−1</sup> at a discharge current density of 0.1 A g<sup>−1</sup>, increasing the active material utilization to 69.6% of theoretical capacity. In addition, the batteries maintained a discharge capacity of 152 mAh g<sup>−1</sup> after 800 cycles, with a capacity retention rate of 91%, which is better than most pre-reported values. The charging and discharging mechanisms of the positive electrode were analyzed using Raman, X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, and transmission electron microscopy.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"60 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140930958","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-06DOI: 10.1007/s00706-024-03207-2
Majid Yaghoubi, Ali Reza Zanganeh, Nader Mokhtarian, Mohammad Hassan Vakili
In this work, a sensing platform founded on the immobilization of ZIF-67 and rGO nanocomposite (ZIF-67/rGO) by Nafion on the glassy carbon electrode surface was fabricated and used for probing silver by differential pulse anodic stripping voltammetry (DPASV) procedure. The half-fraction central composite design (HF-CCD) was utilized for optimizing the experimental variables (weight percentage of composite: 8%; pre-concentration time and applied potential: 240 s, −1.3 V; scan rate of DPASV: 100 mV s−1; pre-concentration solution pH: 6). The detection limit was 4.0 × 10−11 mol/dm3. The repeatability (relative standard deviation) of the measurements using a single sensor was approximately 4% (n = 5, 1.0 × 10−8 mol/dm3 Ag(I)). One of the advantages of the proposed sensor is its high selectivity, which is based on the size-selective property of the ZIF-67 toward silver, and it causes the interference of other species, especially mercury, to be absent. Also, the use of Nafion immobilizes a large amount of composite on the surface of the electrode, and on the other hand, the synergistic effect related to the high conductivity of rGO and the high porosity of the ZIF-67 causes effective pre-concentration of silver by the composite, and these two factors strengthen the sensor signal, increase sensitivity and cause reaching the appropriate detection limit. In this research, an attempt has been made to overcome the challenges of using ZIF-67 in the construction of an electrochemical sensor, and its results can be used to build electrochemical platforms based on MOFs.
{"title":"Nanocomposite of ZIF-67/reduced graphene oxide as sensing element for voltammetric detection of silver(I) ion: optimizing operational conditions by half-fraction central composite design","authors":"Majid Yaghoubi, Ali Reza Zanganeh, Nader Mokhtarian, Mohammad Hassan Vakili","doi":"10.1007/s00706-024-03207-2","DOIUrl":"https://doi.org/10.1007/s00706-024-03207-2","url":null,"abstract":"<p>In this work, a sensing platform founded on the immobilization of ZIF-67 and rGO nanocomposite (ZIF-67/rGO) by Nafion on the glassy carbon electrode surface was fabricated and used for probing silver by differential pulse anodic stripping voltammetry (DPASV) procedure. The half-fraction central composite design (HF-CCD) was utilized for optimizing the experimental variables (weight percentage of composite: 8%; pre-concentration time and applied potential: 240 s, −1.3 V; scan rate of DPASV: 100 mV s<sup>−1</sup>; pre-concentration solution pH: 6). The detection limit was 4.0 × 10<sup>−11</sup> mol/dm<sup>3</sup>. The repeatability (relative standard deviation) of the measurements using a single sensor was approximately 4% (<i>n</i> = 5, 1.0 × 10<sup>−8</sup> mol/dm<sup>3</sup> Ag(I)). One of the advantages of the proposed sensor is its high selectivity, which is based on the size-selective property of the ZIF-67 toward silver, and it causes the interference of other species, especially mercury, to be absent. Also, the use of Nafion immobilizes a large amount of composite on the surface of the electrode, and on the other hand, the synergistic effect related to the high conductivity of rGO and the high porosity of the ZIF-67 causes effective pre-concentration of silver by the composite, and these two factors strengthen the sensor signal, increase sensitivity and cause reaching the appropriate detection limit. In this research, an attempt has been made to overcome the challenges of using ZIF-67 in the construction of an electrochemical sensor, and its results can be used to build electrochemical platforms based on MOFs.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"16 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140930833","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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