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21.
Yulia B. Monakhova Svetlana P. Mushtakova Thomas Kuballa Dirk W. Lachenmeier 《Magnetic resonance in chemistry : MRC》2014,52(12):755-759
An eight‐fold suppression pulse sequence was recently developed to improve sensitivity in 1H NMR measurements of alcoholic beverages [Magn. Res. Chem. 2011 (49): 734–739]. To ensure that only one combined hydroxyl peak from water and ethanol appears in the spectrum, adjustment to a certain range of ethanol concentrations was required. To explain this observation, the structure of water–ethanol solutions was studied. Hydroalcoholic solutions showed extreme behavior at 25% vol, 46% vol, and 83% vol ethanol according to 1H NMR experiments. Near‐infrared spectroscopy confirmed the occurrence of four significant compounds (‘individual’ ethanol and water structures as well as two water–ethanol complexes of defined composition – 1 : 1 and 1 : 3). The successful multiple suppression can be achieved for every kind of alcoholic beverage with different alcoholic strengths, when the final ethanol concentration is adjusted to a range between 25% vol and 46% vol (e.g. using dilution or pure ethanol addition). In this optimum region, an individual ethanol peak was not detected, because the ‘individual’ water structure and the 1 : 1 ethanol–water complex predominate. The nature of molecular association in ethanol–water solutions is essential to elucidate NMR method development for measurement of alcoholic beverages. The presented approach can be used to optimize other NMR suppression protocols for binary water–organic solvent mixtures, where hydrogen bonding plays a dominant role. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
22.
Kirill V. Zaitsev Yulia A. Piskun Yuri F. Oprunenko Sergey S. Karlov Galina S. Zaitseva Irina V. Vasilenko Andrei V. Churakov Sergei V. Kostjuk 《Journal of polymer science. Part A, Polymer chemistry》2014,52(9):1237-1250
The aluminum complexes containing two iminophenolate ligands of the type (p‐XC6H4NCHC6H4O‐o)2AlR' (R′=Me ( 3, 4 ) or R′=O(CH2)4OCH=CH2 ( 5, 6 ), X=H ( 3, 5 ), F( 4, 6 )) were synthesized and characterized by 1H, 13C NMR spectroscopy, and X‐ray crystallography. The reaction of AlMe3 with two equivalents of substituted iminophenols gave five‐coordinated {ONR}2AlMe ( 3, 4 ) complexes. Subsequent reaction of these methyl complexes with unsaturated alcohol, HO(CH2)4OCH=CH2, resulted in target compounds 5 and 6 in a good yield. It was shown that the complexes ( 3 ‐ 6 ) are monomeric in solution (NMR) and in solid state (X‐ray analysis). The catalytic activity of the complexes 5 and 6 towards ring‐opening polymerization (ROP) of ?‐caprolactone and d,l ‐lactide was assessed. Complex 5 showed higher activity as compared with 6 , while both of these catalysts induced controlled homo‐ and copolymerization to afford the macromonomers with high content of vinyl ether end groups (Fn > 80%) in a broad range of molecular weights (Mn = 4000–30,000 g mol?1) with relatively narrow MWD (Mw/Mn = 1.1–1.5). © 2014 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 1237–1250 相似文献
23.
Design of pincer complexes based on (methylsulfanyl)acetic/propionic acid amides with ancillary S‐ and N‐donors as potential catalysts and cytotoxic agents 下载免费PDF全文
Svetlana G. Churusova Diana V. Aleksanyan Andrei A. Vasil'ev Ekaterina Yu. Rybalkina Olga Yu. Susova Zinaida S. Klemenkova Rinat R. Aysin Yulia V. Nelyubina Vladimir A. Kozlov 《应用有机金属化学》2018,32(6)
Pincer complexes featuring readily tunable tridentate ligand frameworks comprise one of the most actively studied classes of organometallic and metal–organic compounds and find extensive use in catalysis, organic synthesis, materials science, and other fields of chemistry and allied disciplines. Currently growing attention is devoted to non‐classical ligand scaffolds, such as functionalized carboxamides, which offer multiple options for directed structural modifications. In this study, the reactions of (methylsulfanyl)acetyl and propanoyl chlorides with 2‐(aminomethyl)pyridine, 2‐(2‐aminoethyl)pyridine, 8‐aminoquinoline and 2‐(diphenylthiophosphoryl)aniline afford a series of new pincer‐type ligands based on functionalized carboxamides. The ligands obtained readily undergo direct cyclopalladation under the action of PdCl2(NCPh)2 in dichloromethane at room temperature, resulting in Pd(II) pincer complexes with N,N,S‐ and S,N,S‐donor sets. Importantly, some of the cyclopalladated derivatives can also be produced efficiently under solvent‐free conditions according to the approach recently developed by our group. The complexes obtained have been tested for cytotoxicity against several human cancer cell lines and catalytic activity in the model Suzuki reaction. The results have been compared to those for the related Pd(II) pincer complexes to define the main structure–activity relationships and to outline the most promising structures for further investigations. 相似文献
24.
Margarita Yu. Vozhdaeva Alfiya R. Kholova Igor A. Melnitskiy Ilya I. Beloliptsev Yulia S. Vozhdaeva Evgeniy A. Kantor Albert T. Lebedev 《Molecules (Basel, Switzerland)》2021,26(7)
The main drawback of drinking water chlorination involves the formation of quite hazardous disinfection by-products (DBPs), represented mainly by halogenated species. Based on the authors’ monitoring data since 2002, the prevalence of chlorine over bromine in the composition of volatile DBPs was shown for the drinking water in Ufa (Russia). However, the situation was completely reversed in the case of semi-volatile DBPs. The principal goal of the present study involved rationalization of the results of the long-term monitoring. Gas chromatography–mass spectrometry (GC-MS) was used for the qualitative and quantitative analysis of volatile DBPs. Identification of semi-volatile compounds was carried out with GC-MS, while gas chromatography with an atomic emission detector (GC-AED) was used for their quantification. A significant contribution of oxygen to the composition of semi-volatile compounds proves the decisive role of the dissolved organic matter oxidative destructive processes. Statistical analysis revealed notable linear correlations for trihalomethane and haloacetic acid formation vs. chlorine dose. On the contrary, halogenated semi-volatile products do not demonstrate any correlations with the water quality parameters or chlorine dose. Principal component analysis (PCA) placed them into separate groups. The results allow for proposing that formation of the organohalogenated species involved the fast penetration of bromine into the humic matter molecules and, further, their oxidative destruction by active chlorine. 相似文献
25.
Dr. Anton A. Anisimov Dr. Fedor V. Drozdov Yulia S. Vysochinskaya Ekaterina O. Minyaylo Prof. Alexander S. Peregudov Prof. Fedor M. Dolgushin Dr. Olga I. Shchegolikhina Prof. Aziz M. Muzafarov 《Chemistry (Weinheim an der Bergstrasse, Germany)》2020,26(50):11404-11407
This study presents the synthesis of organoboron derivatives of stereoregular 4-, 6-, and 12-unit phenylcyclosilsesquioxanes. All compounds obtained were isolated in good yields (70–80 %) and were fully characterized by 1H, 13C, 29Si, 11B NMR, IR spectroscopy, HRMS ESI, and elemental microanalysis. The structure of the key modifier, obtained for the first time, 4-(tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl) dimethylvinylsilane, was also confirmed by single-crystal XRD. 相似文献
26.
27.
Elena B. Averina Yuri V. Samoilichenko Yulia A. Volkova Yuri K. Grishin Victor B. Rybakov Andrei G. Kutateladze Mikhail E. Elyashberg Tamara S. Kuznetsova Nikolai S. Zefirov 《Tetrahedron letters》2012,53(12):1472-1475
Revised regiochemistry for the heterocyclization of electrophilic alkenes with tetranitromethane (TNM) in the presence of triethylamine, providing rapid access to nitroisoxazoles, is reported. The formation of 5-nitroisoxazoles previously incorrectly assigned as 3-nitro regioisomers, has now been established unambiguously by X-ray crystallography. Empirical computations with ACD/CNMR Predictor, based both on hierarchical ordering of spherical environments (HOSE) and an algorithm of artificial neural networks (ANN), and also Density Functional Theory computations of the 13C NMR chemical shifts for the 3- versus 5-nitroisoxazoles are shown to consistently match the spectra of the experimentally observed 5-regioisomers. 相似文献
28.
Almaz Zagidullin Yulia Ganushevich Vasili Miluykov Oleg Sinyashin Evamarie Hey-Hawkins 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-3):238-242
Abstract The reactivity of 1-alkyl-1,2-diphospholes in cycloaddition reactions with dienes, dienophiles or 1,3-dipoles was examined. 1-Alkyl-1,2-diphospholes (2 ) exhibit dual reactivity and act as diene toward maleic acid derivatives or as dienophiles with 2,3-dimethyl-1,3-butadiene. The 1-alkenyl-1,2-diphospholes (4 ) are readily involved in intramolecular [4 + 2] cycloaddition reactions leading to cage phosphines (5 ). Interaction of 1-alkyl-1,2-diphospholes (2) with 1,3-dipolar reagents (diphenyldiazomethane and nitrones) results in formation of the bicyclic phosphiranes (8) and dimers of 1-alkyl-1,2-diphosphole oxides (9) or bicyclic phosphine oxides (10) with a β-lactam moiety depending on temperature. 相似文献
29.
Dmitry V. Pankratov Yulia S. Zeifman Olga V. Morozova Galina P. Shumakovich Irina S. Vasil'eva Sergey Shleev Vladimir O. Popov Alexander I. Yaropolov 《Electroanalysis》2013,25(5):1143-1149
14 Single‐ and multi‐walled carbon nanotubes from different sources were characterized in detail, and the characteristics obtained were carefully analyzed. The carbon material with the highest capacitance, and also other superior properties (“Taunit‐M” from “NanoTechCenter”, Russia), was chosen for further modification and fabrication of buckypaper based electrodes. These electrodes were biomodified with plant and fungal laccases, as well as fungal bilirubin oxidase. The designed biocathodes were investigated in simple buffers and also in a complex physiological fluid (human serum). Biocathodes based on immobilized fungal laccase were bioelectrocatalytically inactive in chloride containing media at neutral pH. In spite of the quite high current densities realized using biodevices based on plant laccase and fungal bilirubin oxidase, the limited thermal stability of the enzymes renders the biocathodes inadequate for practical applications in implanted situations. 相似文献
30.
Denis N. Bazhin Dmitry L. Chizhov Gerd-Volker Röschenthaler Yulia S. Kudyakova Yanina V. Burgart Pavel A. Slepukhin Victor I. Saloutin Valery N. Charushin 《Tetrahedron letters》2014
1,1,1-Trifluoro-4,5,5-trimethoxyhex-3-en-2-one and lithium (2Z)-1,1,1-trifluoro-5,5-dialkoxy-4-oxohex-2-en-2-olate were synthesized for the first time via direct trifluoroacetylation of 2,3-butanedione acetal derivatives. A simple and effective approach to acetal or acyl substituted CF3-pyrazoles, 5,5′-bis(trifluoromethyl)-3,3′-bipyrazole, and, to 5-trifluoromethylfuran-3-ones is presented. 相似文献