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Journal articles on the topic 'Lc-Hrms2 | 13c nmr'

Author: Grafiati

Published: 7 July 2024

Last updated: 31 July 2025

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1

Jankowski, C. K., M. R. Van Calsteren, N. Aychet, J. F. Dozol, C. Moulin, and C. Lamouroux. "Study of the nitration of di-n-octylcrown-6 calix[4]arene using LCMS, NMR, and molecular modelling." Canadian Journal of Chemistry 83, no. 8 (2005): 1098–113. http://dx.doi.org/10.1139/v05-126.

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The selective HNO3 nitration of di-n-octylcrown-6 calix[4]arene using different conditions, studied with LCMS and NMR (1H and 13C) spectroscopic techniques, lead to the identification of most of the expected nitro derivative isomeric compounds. The formation of these isomers under acidic and radiolytic conditions is discussed with the help of molecular modelling.Key words: calix crown compounds, nitration of calixarenes, NMR of isomeric nitrocalixarenes, LC-ESI-MS.

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2

Shupeniuk, Vasyl, Tetyana Taras, Oksana Sabadakh, Eugene Luchkevich, and Yurii Kornii. "Synthesis some 4-substituted 9,10-anthraquinones." French-Ukrainian Journal of Chemistry 8, no. 1 (2020): 58–65. http://dx.doi.org/10.17721/fujcv8i1p58-65.

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New 4-substituted 9,10-anthraquinones (6 compouds) with amino derivations fragments were synthesized through the substitution of the bromaminic acid by amines using the Ullmann coupling reaction. The structures of the synthesized compounds were determined using LC-MS, 1H NMR, 13C NMR spectroscopy, and elemental analysis data.

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3

Kerschl, Susanna, and Bernd Wrackmeyer. "Notizen: Versuche zur Herstellung eines Alkenyl(dimethyl)zinnhydrids: Gibt es eine intramolekulare Sn–H–B-Brücke?/ Attempts at the Synthesis of an Alkenyl(dimethyl)tin Hydride: Is there an Intramolecular Sn–H–B Bridge?" Zeitschrift für Naturforschung B 42, no. 8 (1987): 1047–49. http://dx.doi.org/10.1515/znb-1987-0820.

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Abstract2-(E)-Dim ethyl(chloro)stannyl-3-diethylboryl-2- pentene (lc) reacts with trimethyltin hydride (3) to give the corresponding alkenyl(dim ethyl)tin hydride (2). Compound 2 has been characterized by 1H, 11B, 13C, 119Sn NMR . Neither the NMR nor the IR data are in support of an intramolecular Sn-H-B bridge.

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4

Xie, Yimin, Xudong Chen, Kai Zhang, Sheng Cui, and Gongxia Zhang. "Elucidation of lignin and polysaccharide linkages in wheat straw by 2H/13C isotopic tracer." BioResources 18, no. 1 (2022): 550–69. http://dx.doi.org/10.15376/biores.18.1.550-569.

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To elucidate chemical linkages between lignin and polysaccharides, the aqueous mixed solutions of coniferin-[α-13C], syringin-[α-13C], D-glucose-[6-2H], and phenylalanine ammonia-lyase inhibitor were injected into a living wheat stalk. Internode tissues with high abundance of 2H-13C were collected. The milled wood lignin, lignin-carbohydrate complex (LCC), and residual LCC (R-LCC) with enrichment of 2H-13C were isolated. The 13C and 2H abundances showed that the lignin and polysaccharides of internode tissues were labeled by 13C and 2H, respectively. Analysis with carbon-13 nuclear magnetic re

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5

Fiadorwu, Joshua, Kiran Subedi, Daniel Todd, and Mufeed M. Basti. "Multipronged Approach to Profiling Metabolites in Beta vulgaris L. Dried Pulp Extracts Using Chromatography, NMR and Other Spectroscopy Methods." Foods 12, no. 18 (2023): 3510. http://dx.doi.org/10.3390/foods12183510.

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Beetroot (Beta vulgaris L.) is known for being a rich source of phytochemicals, minerals and vitamins. This study aims to show how the combination of extraction/chromatography/mass spectrometry and NMR offers an efficient way to profile metabolites in the extracts of beetroot. Such combination may lead to the identification of more nutritional or medicinal compounds in natural products, and it is essential for our ongoing investigation to study the selective adsorption/desorption of these metabolites’ on/off nanoparticles. The aqueous and organic extracts underwent analyses using UV-vis spectr

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6

Bhaskar, Prakash, Vasantha Kumar, Suresha Kumara Tholappanavara Hanumanthappa, and Sowmya Haliwana Banakara Vijaykumar. "2-(3,4-Dimethoxyphenyl)-N-(4-methoxyphenyl)-1-propyl-1H-benzo[d]imidazole-5-carboxamide." Molbank 2019, no. 3 (2019): M1079. http://dx.doi.org/10.3390/m1079.

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2-(3,4-Dimethoxyphenyl)-N-(4-methoxyphenyl)-1-propyl-1H-benzo[d]imidazole-5-carboxamide was synthesized by the ‘one-pot’ reductive cyclization of N-(4-methoxyphenyl)-3-nitro-4-(propylamino)benzamide with 3,4-dimethoxybenzaldehyde, using sodium dithionite as a reductive cyclizing agent using DMSO as a solvent. The structure of newly synthesized compound was elucidated based on IR, 1H-NMR, 13C-NMR, and LC-MS data.

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7

Bouajila, J., G. Raffin, H. Waton, C. Sanglar, J. O. Païsse, and M. F. Grenier-Loustalot. "Phenolic Resins – Characterizations and Kinetic Studies of Different Resols Prepared with Different Catalysts and Formaldehyde/Phenol Ratios (I)." Polymers and Polymer Composites 10, no. 5 (2002): 341–60. http://dx.doi.org/10.1177/096739110201000502.

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The physicochemical and kinetic properties of resols prepared with different catalysts (NaOH, LiOH and Ba(OH)2) and variable formaldehyde/phenol ratios (2.5 £ R £ 3.5) were followed to determine their effects on the mechanisms and reaction products at a fixed pH and temperature. Kinetic monitoring and quantification of residual monomers were carried out by liquid chromatography coupled with mass spectrometry (LC/UV/MS), by 13C nuclear magnetic resonance (NMR) and by chemical assay for formaldehyde. Oligomer formation (n ≥ 2) was determined by LC/UV/MS, size exclusion chromatography (SEC) and 1

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8

Vasilev, Aleksey A., Peter P. Grozdanov, Ivanka Nikolova, Valentin S. Lozanov, and Meglena I. Kandinska. "Ultrasonic Synthesis and Preliminary Evaluation of Anticoronaviral Activity of 6,7-Dimethoxy-4-(4-(4-methoxyphenyl)piperazin-1-yl)-1-methylquinolin-1-ium Iodide." Molbank 2022, no. 3 (2022): M1400. http://dx.doi.org/10.3390/m1400.

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Quinoline scaffold is one of the most intensively utilized pharmacophores in drug design because of the variety of activities demonstrated by different quinoline-based therapeutics or drug-candidates. Herein, we describe an environmentally tolerant two-step procedure as a convenient synthetic approach to novel chloroquine and hydroxychloroquine analogues. The structures of the newly synthesized compounds are estimated by 1H NMR, 13C NMR, LC-MS spectrometry and IR spectroscopy.

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9

Wojcińska, Małgorzata, Jeffrey Williams, Tom J. Mabry, et al. "Flavonol Triglycosides from the Leaves of Silphium Albiflorum." Natural Product Communications 1, no. 11 (2006): 1934578X0600101. http://dx.doi.org/10.1177/1934578x0600101105.

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In the course of chemotaxonomic studies of the genus Silphium two new and six known flavonol glycosides were isolated from the leaves of S. albiflorum. The structures of the new flavonoids were established by spectral analysis (1H NMR, 13C NMR, HMQC, HMBC, ROESY, TOCSY, MS) as isorhamnetin 3-O-α-L-rhamnosyl (1′“→6″)-O-β-D-galactopyranoside 7-O-β-D-apiofuranoside (1) and quercetin 3-O-α-L-rhamnosyl (1′“→6″)-O-β-D-galactopyranoside 7-O-β-D-apiofuranoside (2). LC-MS and LC-MSn (with post-column manganese complexation) were applied to elucidate the structures of some of the studied compounds.

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10

Canton, Marine, Jane Hubert, Stéphane Poigny, et al. "Dereplication of Natural Extracts Diluted in Glycerin: Physical Suppression of Glycerin by Centrifugal Partition Chromatography Combined with Presaturation of Solvent Signals in 13C-Nuclear Magnetic Resonance Spectroscopy." Molecules 25, no. 21 (2020): 5061. http://dx.doi.org/10.3390/molecules25215061.

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For scientific, regulatory, and safety reasons, the chemical profile knowledge of natural extracts incorporated in commercial cosmetic formulations is of primary importance. Many extracts are produced or stabilized in glycerin, a practice which hampers their characterization. This article proposes a new methodology for the quick identification of metabolites present in natural extracts when diluted in glycerin. As an extension of a 13C nuclear magnetic resonance (NMR) based dereplication process, two complementary approaches are presented for the chemical profiling of natural extracts diluted

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11

Diana, Rosita, Barbara Panunzi та Ugo Caruso. "Two Novel π -Conjugated Fluorophores for Dye-Doped LC On-Off Photoluminescence Switching". Letters in Organic Chemistry 17, № 5 (2020): 340–44. http://dx.doi.org/10.2174/1570178616666191104094527.

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Among various classes of Photoluminescent (PL) compounds, soft-matter based materials in which chromophores are embedded in a Liquid-Crystal (LC) host polymer prove to be very attractive in the production of flexible panels and on-off temperature switches. Actually, the obtainment of low cost, easily synthesizable, and stable organic molecules soluble in the LC matrix is a challenge for both scholars and technologists. Here we describe the synthesis of two new emissive dyes based on a dicyanophenylenevinylene and on a bis-azobenzene core whose PL properties were investigated as neat solids, in

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12

Kumar, Rakesh, and Gursharan Singh. "Reactions of MoCl5 with 4-Methylpyridine, 2-Methylpyridine and 1-Methylimidazole in Tetrahydrofuran." Oriental Journal Of Chemistry 37, no. 5 (2021): 1178–86. http://dx.doi.org/10.13005/ojc/370523.

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MoCl5 reactions with 4-methylpyridine/2-methylpyridine/1-methylimidazole in THF in 1:1/1:2 stoichiometric ratios, at room temperature were carried out. The following products were synthesized: MoO2Cl(C6H7N), 1;Mo2O2Cl5(C6H7N)2(C4H8O)2,2; Mo4O4Cl4(C6H7N)3(C4H8O)2, 3 and Mo2O4Cl4(C4H6N)2(C4H8O), 4. These compounds have been investigated by FT-IR (transmission mode), FT-1H NMR, FT -13C NMR, microbiological, LC-MS and elemental (C, H, N, Mo, Cl) studies. In view of the sensitivity of all the reactants and products towards oxidation/hydrolysis by air/moisture, all the reactions and products were ha

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13

Gurav, M. M., R. M. Tigote, and A. W. Suryawanshi. "Magnetically Recoverable Fe0.02Zn0.95-xCr0.05O Iron doped Catalyst for Synthesis of Dihydropyrimidones, Thiones and their Derivatives." Asian Journal of Chemistry 34, no. 12 (2022): 3247–50. http://dx.doi.org/10.14233/ajchem.2022.24043.

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A new technique for the impregnation of magnetic based catalyst component onto the organic molecules are widely discussed. Due to its benefits of high surface area, separation simplicity, recyclability and limited leaching of catalytic active ingredients from the catalyst, in the present work, iron-doped Fe0.02Zn0.95-xCr0.05O heterogeneous catalyst was applied in the synthesis of dihydropyrimidones, thiones and their derivatives. The synthesized compounds were elucidated by their IR, 1H NMR and 13C NMR and LC-MS analysis.

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14

Fujiwara, Tao, Ayumi Uehara, Junichi Kitajima, Tsukasa Iwashina, Sadamu Matsumoto, and Yasuyuki Watano. "Genkwanin 4′-O-glucosyl-(1→2)-rhamnoside from New Chemotype of Asplenium normale in Japan." Natural Product Communications 9, no. 9 (2014): 1934578X1400900. http://dx.doi.org/10.1177/1934578x1400900917.

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New flavone glycoside, genkwanin 4′- O-β-glucopyranosyl-(1→2)- O-α-rhamnopyranoside was isolated from the fronds of new chemotype of Asplenium normale D.Don, together with two known C-glycosylflavones, vicenin-2 and lucenin-2. The chemical structure of the isolated glycoside was established by UV, LC-MS, characterization of acid hydrolysates, and 1H and 13C NMR spectroscopy.

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15

Manoharan, Dhinesh kumar. "Synthesis, Characterization and Evaluation of Anti-inflammatory Activity of Novel Indoline Derivatives." JOURNAL OF ADVANCES IN CHEMISTRY 12, no. 12 (2016): 4557–63. http://dx.doi.org/10.24297/jac.v12i12.4826.

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Series of indoline derivatives were synthesized using N-(4-aminophenyl) indoline-1-carbothiamide as a precursor. The structures of synthesized compounds were confirmed by FT-IR, 1H-NMR, 13C-NMR and LC-MS. The in vitro anti-inflammatory activity of synthesized indoline derivatives were examined by standard anti-denaturation assay. The compounds 4a (IC50 = 62.2 µg/ml) and 4b (IC50 = 60.7 µg/ml) showed potent inhibition on protein denaturation. The compounds 5a (IC50 = 97.8 µg/ml) exhibits moderate inhibition on protein denaturation

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16

Asquith, Christopher, and Graham Tizzard. "6-Bromo-N-(2-methyl-2H-benzo[d][1,2,3]triazol-5-yl)quinolin-4-amine." Molbank 2019, no. 4 (2019): M1087. http://dx.doi.org/10.3390/m1087.

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We describe a straightforward synthesis of the title compound, incorporating a relatively rare 2-methyl-2H-1,2,3-triazole heterocylic motif as a potential kinase inhibitor motif. The small molecule crystal structure has been resolved, revealing an interesting packing arrangement and overall conformation. We also performed routine characterization with 1H/13C-NMR and liquid chromatography (LC) and high-resolution mass spectra (HRMS).

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17

Krska, Rudolf, Elvira Welzig, Ralf D. Josephs, et al. "Purity Assessment of Crystalline Zearalenone." Journal of AOAC INTERNATIONAL 86, no. 4 (2003): 722–28. http://dx.doi.org/10.1093/jaoac/86.4.722.

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Abstract Commercially available solid zearalenone (ZON) to be used as a certified liquid calibrant (BCR-699) in a project funded by the European Commission within the Standard Measurement and Testing program was characterized and its purity determined. The degree of purity of the ZON was examined by UV spectrophotometer, liquid chromatography (LC) with diode array and fluorescence detection, 1H and 13C-NMR spectrometry, LC–mass spectrometry (LC/MS/MS), ion chromatography (IC), and differential scanning calorimetry (DSC). The diagrams obtained from DSC analysis and the UV spectrum showed no det

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18

Moriyasu, Takako, Keiko Minowa, Miho Sakamoto, et al. "Differentiation Between Sulfoaildenafil and Its Analogs." Journal of AOAC INTERNATIONAL 94, no. 6 (2011): 1770–77. http://dx.doi.org/10.5740/jaoacint.10-425.

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Abstract An analog of aildenafil, which is a potent and highly selective inhibitor of phosphodiesterase 5, was found in a dietary supplement marketed for enhancement of sexual function. The compound was isolated by silica gel column chromatography, and its structure was identified by means of 13C-NMR spectrometry, 1H-NMR spectrometry, high-resolution MS, and X-ray structure determination. The compound was identified to be sulfoaildenafil (other names: thioaildenafil, dimethyl sildenafil thione, and thiomethisosildenafil). Sulfoaildenafil is very similar to the compound thiohomosildenafil. As i

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19

Wang, Qing, Huang Chen, Hao Xing, Yuan Deng, Zhi-Wang Luo, and He-Lou Xie. "Long Rod-Like Liquid Crystal Containing Azobenzene and the Applications in Phase-Transition Regulation and Orientation of Nematic Liquid Crystal." Crystals 11, no. 4 (2021): 418. http://dx.doi.org/10.3390/cryst11040418.

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Phase-transition and orientation of liquid crystal (LC) are two crucial factors for LC application. In this work, a long rod-like LC compound containing double azobenzene (M1) is successfully designed and synthesized. The combing technologies of nuclear magnetic resonance (1H NMR, 13C NMR) and Fourier transform infrared spectroscopy (FTIR) are used to identify the chemical structure of the molecule. Additionally, the polarized optical microscopy (POM), differential scanning calorimetry (DSC), and one-dimensional wide-angle X-ray diffraction (1D WAXD) experimental results show that M1 exhibits

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20

Wecksler, Aaron T., Victor Lundin, Ambrose J. Williams, Karthik Veeravalli, Dorothea E. Reilly, and Sung-Hye Grieco. "Bioprocess Development and Characterization of a 13C-Labeled Hybrid Bispecific Antibody Produced in Escherichia coli." Antibodies 12, no. 1 (2023): 16. http://dx.doi.org/10.3390/antib12010016.

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Monoclonal antibodies (mAbs) are highly efficacious therapeutics; however, due to their large, dynamic nature, structural perturbations and regional modifications are often difficult to study. Moreover, the homodimeric, symmetrical nature of mAbs makes it difficult to elucidate which heavy chain (HC)-light chain (LC) pairs are responsible for any structural changes, stability concerns, and/or site-specific modifications. Isotopic labeling is an attractive means for selectively incorporating atoms with known mass differences to enable identification/monitoring using techniques such as mass spec

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21

Sowmya, P. T., and K. M. Lokanatha Rai. "Synthesis and Liquid Crystalline Properties of a New Homologous Series of 4,5-Disubstituted 2H-[1,2,3]-Triazoles via Azide-Chalcone Oxidative Cycloaddition Reaction." Australian Journal of Chemistry 70, no. 7 (2017): 764. http://dx.doi.org/10.1071/ch16540.

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A new homologous series of 4,5-disubstituted 2H-[1,2,3]-triazole derivatives were synthesized from chalcones and sodium azide via oxidative cycloaddition reaction; CuI was used as catalyst. Flexibility in the synthesized molecules was provided by attaching straight alkoxy chains. The synthesized compounds were characterized by elemental analysis, and 1H NMR and 13C NMR and LC-MS spectroscopies . The stability and range of the mesophases increased with the length of the chain on the triazoles. The melting point, transition temperatures, and enantiotropic liquid crystal morphologies were determi

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22

Alqudah, Enas, Malak Abbadi, Sawsan Alqadoomi, Ibtihal Abo Hameda, Sharif Arar, and Kamal Sweidan. "Identification and Separation of the Degradation Products of Vildagliptin Tablets and Raw Material using LC-MS and NMR, and then Exploration of the Corresponding Degradation Pathways." Jordan Journal of Pharmaceutical Sciences 16, no. 2 (2023): 478. http://dx.doi.org/10.35516/jjps.v16i2.1535.

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A gradient high performance liquid chromatography (HPLC) method has been developed for the qualitative and quantitative analyses of vildagliptin related substances. This method is based on using of RP-C18 (250 × 4.6 mm×5µm) and gradient elution with phosphate buffer and methanol as mobile phase. Various forced degradation studies were conducted to establish an impurity profile for vildagliptin in the tablet formula. Three degradation products were produced upon exposing vildagliptin to different degradation conditions (acidic, basic, oxidative, photolytic, aqueous and thermal); their structure

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23

Sakaguchi, Keisuke, Junichi Kitajima, and Tsukasa Iwashina. "Kaempferol Tri- and Tetraglycosides from the Flowers of Clematis Cultivar." Natural Product Communications 7, no. 2 (2012): 1934578X1200700. http://dx.doi.org/10.1177/1934578x1200700210.

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A new kaempferol glycoside, kaempferol 3- O-α-rhamnopyranosyl-(1→2)-[α-rhamnopyranosyl-(1→6)-β-glucopyranoside]-7- O-β-glucopyranoside (2) was isolated from the flowers of Clematis cultivar “Jackmanii Superba”, together with a known kaempferol 3- O-α-rhamnopyranosyl-(1→6)-β-glucopyranoside-7- O-β-glucopyranoside (1). The chemical structures of the isolated glycosides were established by UV, LC-MS, characterization of acid hydrolysates, and 1H and 13C NMR spectroscopy.

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24

Bhupatiraju, Rajesh Varma, Battula Sreenivasa Rao, Kapavarapu Maruthi Venkata Narayana Rao, and Mandapati Varaprasad Reddy. "A NOVEL RIVAROXABAN DEGRADATION IMPURITY DETECTION BY RP-HPLC, EXTRACTION BY PREPARATORY CHROMATOGRAPHY, AND CHARACTERIZATION BY LCMS, NMR, AND FT-IR: ANALYSIS OF NOVEL IMPURITY IN BATCH SAMPLES AND TABLETS OF RIVAROXABAN." RASAYAN Journal of Chemistry 15, no. 04 (2022): 2373–81. http://dx.doi.org/10.31788/rjc.2022.1547008.

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A novel rivaroxaban degradant was obtained at 0.45% w/w level during the “RP-HPLC” analysis in the acetic acidexposed rivaroxaban sample. This novel rivaroxaban degradant has a relative retention period (RRT) of approximately 0.95 min. This 0.95 RRT impurity was recognized by LC-MS and then characterized by 1H NMR, 13C NMR, NMR HSQC, NMR HMBC and NMR D2O exchange analyses, and FT-IR techniques. Employed Zorbax XDB C18 eclipse as the main column and Ghost-Guard-LC, ANP00001 as the Ghostbuster column for 0.95 RRT molecule analysis. The mobile phase, phosphate buffer, and acetonitrile mixture, wi

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25

S. TirumalaJagadeesh and N.V.S.Venugopal. "DESIGNED SYNTHESIS AND BIOEVOLUTION OF A NOVEL ANALOGOUS OF THIADIAZOLO [3, 2-A] PYRIMIDINE-6- CARBOXYLATE PROMOTED BY TRANSITION METAL ACETATES." RASAYAN Journal of Chemistry 18, no. 03 (2025): 1252–60. https://doi.org/10.31788/rjc.2025.1839308.

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In a novel series of [1, 3, 4] thiadiazol-2-amine, a simple new pathway and biological approach, the analogues of Imidazole [3, 2-a] pyrimidine-6-carboxylate (5a-5q). These analogous were obtained by the reaction of intermediate (3) with ethylacetoacetate and substituted aryl aldehydes in the presence of transition metal acetates, while the reaction between thiosemicarbazide and indole-3-carboxylic acid occurs in the presence of protic acid scaffold compound (3). The newly derived compounds are characterised by advanced spectral analysis, including 1H NMR, 13C NMR, and LC-MS. When compared to

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SHARMA, JYOTSNA, HARDEEP SINGH TULI, MAYANK KINGER, RAM PAL, ZAHOOR ABBAS, and MANOJ KUMAR. "Synthesis, Characterization and Biological Screening of Novel Imidazolylpyrazole Scaffolds." Asian Journal of Chemistry 34, no. 3 (2022): 614–18. http://dx.doi.org/10.14233/ajchem.2022.23570.

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A novel series of 3-(4-aryl)-4-(4,5-diphenyl-1H-imidazol-2-yl)-1-phenyl-1H-pyrazole was synthesized by employing the well-known Debus-Radziszewski reaction. Structures of all the newly synthesized compounds have been characterized by various spectroscopic techniques viz. FTIR, 1H and 13C NMR, LC-MS and elemental analysis. All these compounds were also screened for antimicrobial potential against bacterial strains of S. aureus, K. pneumoniae and fungal strains of A. niger and T. rubrum.

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27

Iwashina, Tsukasa, Sadamu Matsumoto, Junichi Kitajima, et al. "Apigenin Di- and Trirhamnoside from Asplenium normale in Malaysia." Natural Product Communications 5, no. 1 (2010): 1934578X1000500. http://dx.doi.org/10.1177/1934578x1000500110.

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Two new flavone rhamnosides, apigenin 7-O-α-L-rhamnopyranosyl-(1→4)-O-α-L-rhamnopyranoside and apigenin 7-O-α-L-rhamnopyranosyl-(1→4)-O-α-L-rhamnopyranoside-4′-O-α-L-rhamnopyranoside were isolated from the fronds of Asplenium normale D. Don, together with two known C-glycosylflavones, vicenin-2 and lucenin-2. The chemical structures of the isolated glycosides were established by UV, LC-MS, characterization of acid hydrolysates, and 1H and 13C NMR spectroscopy.

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LeBlanc, Patricia, Nadine Merkley, Krista Thomas, et al. "Isolation and Characterization of [D-Leu1]microcystin-LY from Microcystis aeruginosa CPCC-464." Toxins 12, no. 2 (2020): 77. http://dx.doi.org/10.3390/toxins12020077.

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[D-Leu1]MC-LY (1) ([M + H]+ m/z 1044.5673, Δ 2.0 ppm), a new microcystin, was isolated from Microcystis aeruginosa strain CPCC-464. The compound was characterized by 1H and 13C NMR spectroscopy, liquid chromatography–high resolution tandem mass spectrometry (LC–HRMS/MS) and UV spectroscopy. A calibration reference material was produced after quantitation by 1H NMR spectroscopy and LC with chemiluminescence nitrogen detection. The potency of 1 in a protein phosphatase 2A inhibition assay was essentially the same as for MC-LR (2). Related microcystins, [D-Leu1]MC-LR (3) ([M + H]+ m/z 1037.6041,

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29

Lou, Rensheng, George Rottinghaus, Andrew L. Thomas, Doug Monroe, Kevin Tran, and Robert E. Smith. "Identification of Unknown Compound in Apocynum cannabinum by High Resolution Mass Spectrometry (HRMS) and 600 MHz NMR." Journal of Regulatory Science 4, no. 3 (2016): 14–19. http://dx.doi.org/10.21423/jrs-v04n03p014.

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High resolution mass spectrometry (HRMS) was able to determine that the m/z of the [M+H]+ ion formed by an unknown compound that was purified by preparative scale liquid chromatography (LC) was 137.05966. This was done rapidly and easily by direct infusion. Neither a column nor chromatography was needed. This is within 0.4 ppm of the mass calculated by ThermoFisher’s exact mass calculator for the protonated version of C8H8O2. Based on this, the compound could have been 2’-, 3’- or 4’-hydroxyacetophenone or 2’-, 3’- or 4’-methoxybenzaldehyde. However, 1H- and 13C-NMR spectra of the isolated com

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Tisserant, Leo-Paul, Jane Hubert, Michelle Lequart, et al. "13C NMR and LC-MS Profiling of Stilbenes from Elicited Grapevine Hairy Root Cultures." Journal of Natural Products 79, no. 11 (2016): 2846–55. http://dx.doi.org/10.1021/acs.jnatprod.6b00608.

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Lee-Chang, Kim Jye, Matthew C. Taylor, Guy Drummond, et al. "Docosahexaenoic Acid Is Naturally Concentrated at the sn-2 Position in Triacylglycerols of the Australian Thraustochytrid Aurantiochytrium sp. Strain TC 20." Marine Drugs 19, no. 7 (2021): 382. http://dx.doi.org/10.3390/md19070382.

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The Labyrinthulomycetes or Labyrinthulea are a class of protists that produce a network of filaments that enable the cells to glide along and absorb nutrients. One of the main two Labyrinthulea groups is the thraustochytrids, which are becoming an increasingly recognised and commercially used alternate source of long-chain (LC, ≥C20) omega-3 containing oils. This study demonstrates, to our knowledge for the first time, the regiospecificity of the triacylglycerol (TAG) fraction derived from Australian thraustochytrid Aurantiochytrium sp. strain TC 20 obtained using 13C nuclear magnetic resonanc

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Holota, Serhii, Ihor Yushyn, Andrzej Gzella, and Roman Lesyk. "3-(2-Diisopropylaminoethyl)-5-(4-methoxybenzylidene)thiazolidine-2,4-dione." Molbank 2022, no. 3 (2022): M1394. http://dx.doi.org/10.3390/m1394.

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Thiazolidine-2,4-dione core is widely used in the medicinal chemistry of different types of potential drug-like small molecules. In the present work, the synthesis of a novel non-condensed thiazolidine-2,4-dione-bearing derivative is reported by the two-step cost-effective approach including alkylation and Knoevenagel condensation. The structure of the synthesized 3-(2-diisopropylaminoethyl)-5-(4-methoxybenzylidene)thiazolidine-2,4-dione was determined and characterized using 1H, 13C NMR, LC-MS spectra and the X-ray diffraction method.

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Madasu, Suri Babu, Nagaji Ambabhai Vekariya, M. N. V. D. Hari Kiran, et al. "Synthesis of compounds related to the anti-migraine drug eletriptan hydrobromide." Beilstein Journal of Organic Chemistry 8 (August 30, 2012): 1400–1405. http://dx.doi.org/10.3762/bjoc.8.162.

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Eletriptan hydrobromide (1) is a selective serotonin (5-HT1) agonist, used for the acute treatment of the headache phase of migraine attacks. During the manufacture of eletriptan hydrobromide the formation of various impurities were observed and identified by LC–MS. To control the formation of these impurities during the preparation of active pharmaceutical ingredients, the structure of the impurities must be known. Major impurities of the eletriptan hydrobromide synthesis were prepared and characterized by using various spectroscopic techniques, i.e., mass spectroscopy, FTIR , 1H NMR, 13C NMR

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Qin, Qiu Yan, Yi Ping Qian, Zi Yu Wang, and Xiao Lin Fan. "Design and Synthesis of Fluorescent Betahistine Conjugates with Unique Imaging Property." Advanced Materials Research 557-559 (July 2012): 712–15. http://dx.doi.org/10.4028/www.scientific.net/amr.557-559.712.

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Labeling cardiovascular drugs probes with a fluorescent tag is an alternative method of measuring drugs activities and distributions in vivo, and further using of advanced tools to diagnose or detect cardiovascular diseases. Using this approach, a fluorescent probe (betahistine-Flu, 1) of Betahistine-based was synthesized and characterized by 1H NMR, 13C NMR and LC-MS, and its UV-Vis absorption spectral and fluorescence spectral, and fluorescence imaging in cell model were investigated. It was found that the fluorescent probe display strong green fluorescence, and have good optical effect in c

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35

Venkataramana, Rupireddy, Venkata Chittireddy, Dongamanti Ashok, and Kudle Rao. "Microwave-assisted synthesis of 2,8-di(alkyl/aryl)-4,6-dichloro-2H,8H-pyrano[3,2-g] chromene-3,7-dicarbaldehydes and their antimicrobial activity." Journal of the Serbian Chemical Society 84, no. 4 (2019): 355–64. http://dx.doi.org/10.2298/jsc180127011v.

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A series of 2,8-di(alkyl/aryl)-substituted bischromanone derivatives were synthesized in one pot from 4,6-diacetylresorcinol and aliphatic/aromatic aldehydes in the presence of pyrrolidine/piperidine under conventional heating and microwave irradiation. The 2,8-di(alkyl/aryl)-substituted bischromanones were converted into a new series of 4,6-dichloro-3,7-diformyl-2,8-di(alkyl/aryl)-substituted bischromenes using the Vilsmeier?Haack reagent. The structures of the compounds were established based on elemental analysis, IR, 1H-NMR, 13C- -NMR and LC?MS spectral data. All the synthesized compounds

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Perike, Nagaraju, Praveen Kumar Edigi, Nirmala Gurrapu, Sridhara Devi Nagulapally, Sushmitha Bujji, and N. J. P. Subhashini. "Synthesis and Characterization of Novel Indole Containing 1,2,3-Triazole Linked 1,3,4-Thiadiazole Hybrids: Evaluation of Anticancer Activity and Molecular Docking Studies." Asian Journal of Chemistry 36, no. 8 (2024): 1946–52. http://dx.doi.org/10.14233/ajchem.2024.32258.

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Novel scaffolds containing indole, 1,2,3-triazole linked thiadiazole derivatives (9a-l) were synthesized and confirmed with analytical techniques like 1H NMR, 13C NMR and LC-MS. All the compounds were further screened for their anticancer activity against two cancer cell lines A-549 and MCF-7 by making use of MTT assay and doxorubicin as standard drug. Among the compounds 9c, 9d and 9e demonstrated prominent activity against the tested cancer cell lines A-549 and MCF-7 cell lines compared to doxorubicin. Auto dock Vina of PyRx tool was employed in order to perform molecular docking studies on

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37

Kovalenko, Drushlyak, Konovalova, et al. "Novel One-Pot Synthesis of Methyl 4-Hydroxy-2-thioxo-1,2-dihydroquinoline-3-carboxylate: Synthetic and Crystallographic Studies." Molbank 2019, no. 4 (2019): M1085. http://dx.doi.org/10.3390/m1085.

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A new suitable method of synthesis of methyl 4-hydroxy-2-thioxo-1,2-dihydroquinoline-3-carboxylate by condensation of methyl 2-isothiocyanatobenzoate and methyl malonate is described. The structure of the compound both and by-product methyl 2(methoxycarbonothioylamino)benzoate was confirmed by means of elemental analysis, 1H NMR, 13C NMR, LC/MS and single crystal X-ray diffraction. UV/Vis and IR spectra of compounds are described. The presence of a strong intramolecular hydrogen bond between the hydroxy group and the carbonyl oxygen atom of the ester group in methyl 4-hydroxy-2-thioxo-1,2-dihy

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Khaniani, Yeganeh, Matthias Lipfert, Dipanjan Bhattacharyya, Rolando Perez Pineiro, Jiamin Zheng, and David Wishart. "A Simple and Convenient Synthesis of Unlabeled and 13C-Labeled 3-(3-Hydroxyphenyl)-3-Hydroxypropionic Acid and Its Quantification in Human Urine Samples." Metabolites 8, no. 4 (2018): 80. http://dx.doi.org/10.3390/metabo8040080.

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An improved method to synthesize the highly abundant and biomedically important urinary metabolite 3-(3-hydroxyphenyl)-3-hydroxypropionic acid (HPHPA) is reported. The modified protocol is based on an indium-mediated sonochemical Reformatsky reaction. The synthesis is a simple two-step route as opposed to a complex four-step route previously reported in the literature that requires specialized equipment, flammable materials, and high-pressure reaction vessels. The described procedure also provides an expedient route to prepare a 13C isotopically labeled HPHPA that can be used as a standard for

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39

Zarev, Yancho, Rada Nedelcheva, Preslav Enchev, Ekaterina Kozuharova, and Iliana Ionkova. "C-glycosylflavones from Linum hologynum Rchb." Pharmacia 72 (February 24, 2025): 1–4. https://doi.org/10.3897/pharmacia.72.e144187.

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The current study focuses on the stem and flowers of Linum hologynum, an endemic species to the Balkan Peninsula, a potential source of valuable metabolites. L. hologynum is poorly studied in any aspects, including its phytochemistry and pharmacological activity. Applying various chromatographic techniques, two isomeric C-glycosylflavones were isolated. Structures were elucidated, by means of spectroscopic methods, including 1H and 13C NMR as well as LC-HRESI-MS analysis, as orientin and isoorientin. This is the first report of those metabolites from L. hologynum.

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Zarev, Yancho. "Isolation and characterization of 3- O-caffeoyloleanolic acid from Robinia pseudoacacia stem bark." Pharmacia 70, no. 4 (2023): 1209–12. http://dx.doi.org/10.3897/pharmacia.70.e110402.

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Robinia pseudoacacia, a deciduous tree native to North America, has various medicinal properties, including antioxidant, antitumour, diuretic and antispasmodic effects. The plant contains various bioactive compounds, such as alkaloids, flavonoids, tannins, and phenols. However, caution is advised as all parts of the plant, except the flowers, are poisonous due to the phytotoxin robinin and its glycoside. The bark, on the other hand, shows resistance to rot due to the antifungal compounds dihydrorobinetin and robinetin. This study focuses on the stem bark of R. pseudoacacia from Bulgaria, a wid

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Iwashina, Tsukasa, Junichi Kitajima, Takayuki Mizuno, Sergey V. Smirnov, Oyunchimeg Damdinsuren, and Katsuhiko Kondo. "New Kaempferol 3,7-Diglycosides from Asplenium ruta-muraria and Asplenium altajense." Natural Product Communications 10, no. 3 (2015): 1934578X1501000. http://dx.doi.org/10.1177/1934578x1501000310.

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A flavonoid was isolated from the fronds of Asplenium ruta-muraria and A. altajense (Aspleniaceae) collected in the Altai Mountains and adjacent area. The compound was identified as kaempferol 3- O- β-[(6″′- E-caffeoylglucopyranosyl)-(1→3)-glucopyranoside]-7- O- β-glucopyranoside (1) by UV, 1H and 13C NMR spectroscopy, LC-MS, and acid and alkaline hydrolyses. Another flavonoid (2) was isolated from A. altajense, as a minor compound, together with 1 and identified as deacylated compound 1, i.e. kaempferol 3- O-laminaribioside-7- O-glucoside. They were found in nature for the first time.

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Murai, Yoshinori, Ryoji Takahashi, Junichi Kitajima, and Tsukasa Iwashina. "New Quercetin Triglycoside from the Leaves of Soybean Cultivar ‘Clark’." Natural Product Communications 14, no. 5 (2019): 1934578X1984361. http://dx.doi.org/10.1177/1934578x19843614.

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A new flavonol triglycoside, Quercetin 3- O-α-rhamnopyranosyl-(1→4)-[α-rhamnopyranosyl-(1→6)-β-galactopyranoside], was isolated from the leaves of soybean ( Glycine max) cultivar “Clark” and identified by UV spectra, LC-ESI-MS, acid hydrolysis, and 1H and 13C NMR. The compound was found together with 7 known flavonol glycosides, quercetin 3- O-robinobioside, quercetin 3- O-rutinoside, kaempferol 3- O-rhamnosyl-(1→4)-[rhamnosyl-(1→6)-galactoside], kaempferol 3- O-robinobioside, kaempferol 3- O-rutinoside, isorhamnetin 3- O-robinobioside, and isorhamnetin 3- O-rutinoside.

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43

Zarev, Yancho, Rada Nedelcheva, Preslav Enchev, Ekaterina Kozuharova, and Iliana Ionkova. "C-glycosylflavones from Linum hologynum Rchb." Pharmacia 72 (February 24, 2025): 1–4. https://doi.org/10.3897/pharmacia.72.e144187.

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The current study focuses on the stem and flowers of <i>Linum hologynum</i>, an endemic species to the Balkan Peninsula, a potential source of valuable metabolites. <i>L. hologynum</i> is poorly studied in any aspects, including its phytochemistry and pharmacological activity. Applying various chromatographic techniques, two isomeric C-glycosylflavones were isolated. Structures were elucidated, by means of spectroscopic methods, including 1H and 13C NMR as well as LC-HRESI-MS analysis, as orientin and isoorientin. This is the first report of those metabolites from <i>L. hologynum</i>.

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44

Cebeci, Yıldız Uygun, and Şengül Alpay Karaoğlu. "Design and microwave-assisted synthesis of a novel Mannich base and conazole derivatives and their biological assessment." Heterocyclic Communications 27, no. 1 (2021): 100–111. http://dx.doi.org/10.1515/hc-2020-0126.

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Abstract 4-Amino-5-methyl-2,4-dihydro-3H-1,2,4-triazol-3-one (1) was converted to the corresponding Schiff base (2) by treatment with salicylaldehyde. 1,2,4-Triazoles were then converted to the corresponding Mannich bases containing fluroquinolone core using a one-pot three-component procedure. Moreover, the synthesis of six compounds, which can be considered as conazole analogues, was performed starting from 1,2,4-triazole-3-one compounds via three steps by either conventional or microwave-mediated conditions. All the newly synthesized compounds were screened for their antimicrobial activitie

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45

Apaydın, Çağla Begüm, Gozde Hasbal Çelikok, and Tuğba Yılmaz Özden. "SYNTHESIS, CHARACTERIZATION AND CHOLINESTERASE INHIBITORY EFFECTS OF IBUPROFEN-BASED SPIROTHIAZOLIDINONES." Ankara Universitesi Eczacilik Fakultesi Dergisi 49, no. 1 (2024): 2. https://doi.org/10.33483/jfpau.1493082.

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Objective: A novel class of spirothiazolidinone derivatives were designed, synthesized, and assessed as possible acetylcholinesterase (AChE) and butyrylcholinesterase (BuChE) inhibitors for Alzheimer's disease therapy. Material and Method: In this study, novel spirocyclic compounds were synthesized by one-pot reaction. IR, 1H NMR, 13C NMR, LC-MS and elemental analysis techniques have all been used to clarify the chemical structures of the compounds. AChE and BuChE inhibitory effects of compounds (4a-e and, 5a-e) were assayed according to Ellman’s method using galantamine as reference. Result a

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46

Veeranki, Krishna Chaitanya, Jalapathi Pochampally, Ravi Chander Maroju, Vishnu Thumma, and Lakshmi Satya Boddu. "1,2,3-Triazoles containing Thiazole-Piperazine Moieties: Synthesis, Biological Assessment and Molecular Docking." Asian Journal of Chemistry 35, no. 1 (2022): 125–34. http://dx.doi.org/10.14233/ajchem.2023.26904.

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A novel series of thiazole-triazole-piperazine multi hybrids was designed for antimicrobial activity and the synthetic method for this series has been developed by copper catalyzed 1,3-dipolar cycloaddition of thiazole-based azide with Boc-piperidine based alkyne in the presence of CuSO4 and sodium ascorbate. Boc deprotection followed by alkylation of piperidine moiety in hybrid derivatives was also carried out. All the target compounds were confirmed using FTIR, 1H NMR, 13C NMR and LC-MS spectral techniques. These compounds were screened for the antimicrobial activity against bacteria and fun

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47

Bouajila, J., G. Raffin, H. Waton, C. Sanglar, J. O. Païsse, and M. F. Grenier-Loustalot. "Phenolic Resins (II) – Influence of the Chemical Structure of High Molecular Weight Molecules on the Mechanisms of Cross-linking and on the Final Structure of the Resins." Polymers and Polymer Composites 11, no. 4 (2003): 233–62. http://dx.doi.org/10.1177/096739110301100401.

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The physicochemical characterization of the structures of the oligomers (n < 4) in resols has been carried out by fragmenting monomers in LC/UV/MS and LC/UV/MS/MS. Fragmentation mechanisms are related to the numbers and positions of substituents on the aromatic ring and to the types of oligomer junctions. It was more difficult to determine the structures of phenol hemiacetals and dimer hemiacetals because of the large number of position isomers. The resols were prepared with differing molar ratios R = Formaldehyde/Phenol and catalysts. They were cross-linked using two industrially recommend

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48

Sato, Moriyuki, Seiji Ujiie, Yuji Tada, and Takashi Kato. "Semirigid Homo- and Copoly(Imide-Carbonate)s Based on 3,4,3″,4″ -p-Terphenyltetracarboxdiimide." High Performance Polymers 10, no. 1 (1998): 155–62. http://dx.doi.org/10.1088/0954-0083/10/1/017.

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Novel thermotropic liquid crystalline (LC) semirigid homo- and copoly(imidecarbonate)s composed of a 3, 4, 3″, 4″- p-terphenyltetracarboxdiimide ring and aliphatic chains were prepared by melt polycondensation of a dihexanol derivative of 3, 4, 3″, 4″- p-terphenyltetracarboxdiimide and/or a dioxydihexanol of biphenyl taken in a definite molar ratio with hexamethylene diphenyl dicarbonate in the presence of zinc acetate, and their thermal and mesogenic properties were evaluated. The assigned structures of polymers were characterized by FT-IR and 13C NMR spectroscopy, and elemental analyses. DSC

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Hryhoriv, Halyna, Illia Mariutsa, Sergiy M. Kovalenko, et al. "The Search for New Antibacterial Agents among 1,2,3-Triazole Functionalized Ciprofloxacin and Norfloxacin Hybrids: Synthesis, Docking Studies, and Biological Activity Evaluation." Scientia Pharmaceutica 90, no. 1 (2021): 2. http://dx.doi.org/10.3390/scipharm90010002.

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Among all modern antibiotics, fluoroquinolones are well known for their broad spectrums of activity and efficiency toward microorganisms and viruses. However, antibiotic resistance is still a problem, which has encouraged medicinal chemists to modify the initial structures in order to combat resistant strains. Our current work is aimed at synthesizing novel hybrid derivatives of ciprofloxacin and norfloxacin and applying docking studies and biological activity evaluations in order to find active promising molecules. We succeeded in the development of a synthetic method towards 1,2,3-triazole-s

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Abadie, Cyril, and Guillaume Tcherkez. "13C Isotope Labelling to Follow the Flux of Photorespiratory Intermediates." Plants 10, no. 3 (2021): 427. http://dx.doi.org/10.3390/plants10030427.

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Measuring the carbon flux through metabolic pathways in intact illuminated leaves remains challenging because of, e.g., isotopic dilution by endogenous metabolites, the impossibility to reach isotopic steady state, and the occurrence of multiple pools. In the case of photorespiratory intermediates, our knowledge of the partitioning between photorespiratory recycling, storage, and utilization by other pathways is thus rather limited. There has been some controversy as to whether photorespiratory glycine and serine may not be recycled, thus changing the apparent stoichiometric coefficient betwee

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