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1.
Poschalko A Lancelot N Marin J Larras V Limal D Elbayed K Raya J Piotto M Briand JP Guichard G Bianco A 《Chemistry (Weinheim an der Bergstrasse, Germany)》2004,10(18):4532-4537
A novel resin called DEUSS (perdeuterated poly(oxyethylene)-based solid support) has been prepared by anionic polymerization of deuterated [D4]ethylene oxide, followed by cross-linking with deuterated epichlorohydrin. DEUSS can be suspended in a wide range of solvents including organic and aqueous solutions, in which it displays a high swelling capacity. As measured by proton HRMAS of the swollen polymer, the signal intensity of the oxyethylene protons is reduced by a factor of 110 relative to the corresponding nondeuterated poly(oxyethylene)poly(oxypropylene) (POEPOP) resin, thus facilitating detailed HRMAS NMR studies of covalently linked molecules. This 1H NMR invisible matrix was used for the solid-phase synthesis of peptides, oligoureas, and a series of amides as well as their characterization by HRMAS NMR spectroscopy. On-bead NMR spectra of high quality and with resolution comparable to that of liquid samples were obtained and readily interpreted. The complete absence of the parasite resin signals will be of great advantage, for example, for the optimization of multistep solid-phase stereoselective reactions, and for the conformational study of resin-bound molecules in a large variety of solvents. 相似文献
2.
Lancelot N Elbayed K Raya J Piotto M Briand JP Formaggio F Toniolo C Bianco A 《Chemistry (Weinheim an der Bergstrasse, Germany)》2003,9(6):1317-1323
A tetra- and a hepta-homopeptide from the C(alpha)-tetrasubstituted Aib (alpha-aminoisobutyric acid) residue were covalently linked to the POEPOP resin by the fragment-condensation approach. The conformational preferences of the two model peptides were determined for the first time on a solid support by means of high-resolution magic angle spinning NMR spectroscopy. The results obtained indicate that the Aib homopeptides adopt a regular 3(10)-helical structure even when they are covalently bound to a polymeric matrix, and thus confirm the remarkable conformational stability of the peptides rich in this amino acid. An ATR-FTIR spectroscopic investigation, performed in parallel, also confirmed that these polymer-bound peptides do indeed adopt a helical conformation. The results of this study open the possibility to exploit the peptide-resin conjugates based on C(alpha)-tetrasubstituted alpha-amino acids as helpful, structurally organized templates in molecular recognition studies or as catalysts in asymmetric synthesis. 相似文献
3.
Role of compositional changes on thermal,magnetic,and mechanical properties of Fe-P-C-based amorphous alloys
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Indah Raya Supat Chupradit Mustafa M Kadhim Mustafa Z Mahmoud Abduladheem Turki Jalil Aravindhan Surendar Sukaina Tuama Ghafel Yasser Fakri Mustafa Alexander N Bochvar 《中国物理 B》2022,31(1):16401-016401
This work aimed to tune the comprehensive properties of Fe-P-C-based amorphous system through investigating the role of microalloying process on the crystallization behavior,glass forming ability(GFA),soft magnetic features,and mechanical properties.Considering minor addition of elements into the system,it was found that the simultaneous microalloying of Ni and Co leads to the highest GFA,which was due to the optimization of compositional heterogeneity and creation of near-eutectic composition.Moreover,the FeCoNiCuPC amorphous alloy exhibited the best anelastic/viscoplastic behavior under the nanoindentation test,which was owing to the intensified structural fluctuations in the system.However,the improved plasticity by the extra Cu addition comes at the expense of magnetic properties,so that the saturation magnetization of this alloying system is significantly decreased compared to the FeCoPC amorphous alloy with the highest soft magnetic properties.In total,the results indicated that a combination of added elemental constitutes,i.e.,Fe69Co5Ni5Cu1P13C7 composition,provides an optimized state for the comprehensive properties in the alloying system. 相似文献
4.
Dr. Isabella A. Vacchi Shi Guo Dr. Jésus Raya Dr. Alberto Bianco Dr. Cécilia Ménard-Moyon 《Chemistry (Weinheim an der Bergstrasse, Germany)》2020,26(29):6591-6598
Graphene oxide (GO) is a versatile platform with unique properties that have found broad applications in the biomedical field. Double functionalization is a key aspect in the design of multifunctional GO with combined imaging, targeting, and therapeutic properties. Compared to noncovalent functionalization, covalent strategies lead to GO conjugates with a higher stability in biological fluids. However, only a few double covalent functionalization approaches have been developed so far. The complexity of GO makes the derivatization of the oxygenated groups difficult to control. The combination of a nucleophilic epoxide ring opening with the derivatization of the hydroxyl groups through esterification or Williamson reaction was investigated. The conditions were selective and mild, thus preserving the structure of GO. Our strategy of double functionalization holds great potential for different applications in which the derivatization of GO with different molecules is needed, especially in the biomedical field. 相似文献
5.
Flavonoid glycosides from Persea caerulea. Unraveling their interactions with SDS‐micelles through matrix‐assisted DOSY,PGSE, mass spectrometry,and NOESY
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Juan M. Álvarez Álvaro Raya‐Barón Pedro M. Nieto Luis E. Cuca Alberto Fernández‐Gutiérrez Ignacio Fernández 《Magnetic resonance in chemistry : MRC》2016,54(9):718-728
Two flavonoid glycosides derived from rhamnopyranoside ( 1 ) and arabinofuranoside ( 2 ) have been isolated from leaves of Persea caerulea for the first time. The structures of 1 and 2 have been established by 1H NMR, 13C NMR, and IR spectroscopy, together with LC–ESI–TOF and LC–ESI–IT MS spectrometry. From the MS and MS/MS data, the molecular weights of the intact molecules as well as those of quercetin and kaempferol together with their sugar moieties were deduced. The NMR data provided information on the identity of the compounds, as well as the α and β configurations and the position of the glycosides on quercetin and kaempferol. We have also explored the application of sodium dodecyl sulfate (SDS) normal micelles in binary aqueous solution, at a range of concentrations, to the diffusion resolution of these two glycosides, by the application of matrix‐assisted diffusion ordered spectroscopy (DOSY) and pulse field gradient spin echo (PGSE) methodologies, showing that SDS micelles offer a significant resolution which can, in part, be rationalized in terms of differing degrees of hydrophobicity, amphiphilicity, and steric effects. In addition, intra‐residue and inter‐residue proton–proton distances using nuclear Overhauser effect build‐up curves were used to elucidate the conformational preferences of these two flavonoid glycosides when interacting with the micelles. By the combination of both diffusion and nuclear Overhauser spectroscopy techniques, the average location site of kaempferol and quercetin glycosides has been postulated, with the former exhibiting a clear insertion into the interior of the SDS‐micelle, whereas the latter is placed closer to the surface. Copyright © 2016 John Wiley & Sons, Ltd. 相似文献
6.
Singh P Toma FM Kumar J Venkatesh V Raya J Prato M Verma S Bianco A 《Chemistry (Weinheim an der Bergstrasse, Germany)》2011,17(24):6772-6780
Single‐walled carbon nanotubes (SWCNTs) have been covalently functionalized with uracil nucleobase. The hybrids have been characterized by using complementary spectroscopic and microscopic techniques including solid‐state NMR spectroscopy. The uracil‐functionalized SWCNTs are able to self‐assemble into regular nanorings with a diameter of 50–70 nm, as observed by AFM and TEM. AFM shows that the rings do not have a consistent height and thickness, which indicates that they may be formed by separate bundles of CNTs. The simplest model for the nanoring formation likely involves two bundles of CNTs interacting with each other via uracil–uracil base‐pairing at both CNT ends. These nanorings can be envisaged for the development of advanced electronic circuits. 相似文献
7.
Philippe Bertani Jsus Raya Pierre Reinheimer Rgis Gougeon Luc Delmotte Jrme Hirschinger 《Solid state nuclear magnetic resonance》1999,13(4):255-229
19F/29Si Hartmann–Hahn continuous wave cross-polarization (CP) has been applied under fast magic-angle spinning (MAS) to a powder sample of octadecasil. Strong oscillations occur during CP on a sideband matching condition between the isolated 29Si–19F spin pairs formed by the silicons in the D4R units and the fluoride anions. The magnitude of the dipolar coupling constant was deduced directly from the line-splitting between the intense singularities of the Pake-like patterns obtained by Fourier transformation of the oscillatory polarization transfer. The corresponding Si–F internuclear distance, r=2.62±0.05 Å, is found to be in very good agreement with the X-ray crystal structure and the value of 2.69±0.04 Å recently reported from rotational echo double resonance (REDOR) and transferred echo double resonance (TEDOR) nuclear magnetic resonance (NMR) experiments. Furthermore, the CP technique is still reliable under fast MAS where both REDOR and TEDOR sequences suffer from severe artefacts due to finite pulse lengths. In octadecasil, a spinning frequency of 14 kHz is shown to be necessary for an effective suppression of 19F–19F spin diffusion. The influences of experimental missettings and radiofrequency (RF) field inhomogeneity are taken into account. 相似文献
8.
The fermion propagator in an arbitrary covariant gauge can be obtained from the Landau gauge result via a Landau–Khalatnikov–Fradkin
transformation. This transformation can be written in a practically useful form in both configuration and momentum space.
It is therefore possible to anticipate effects of a gauge transformation on the propagator’s analytic properties. These facts
enable one to establish that if a critical number of flavours for chiral symmetry restoration and deconfinement exists in
noncompact QED3, then its value is independent of the gauge parameter. This is explicated using simple forms for the fermion–photon
vertex and the photon vacuum polarisation. The illustration highlights pitfalls that must be avoided in order to arrive at
valid conclusions. Landau gauge is seen to be the covariant gauge in which the propagator avoids modification by a non-dynamical
gauge-dependent exponential factor, whose presence can obscure truly observable features of the theory. 相似文献
9.
Sonia Ovarlez Dr. Françoise Giulieri Dr. Anne‐Marie Chaze Prof. François Delamare Prof. Jesus Raya Dr. Jerome Hirschinger Dr. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2009,15(42):11326-11332
Evidence for access of molecules the size of acetone or pyridine to the intracrystalline tunnels of nanofibre clay (sepiolite) has indicated formation of a new type of organic–inorganic nanocomposites. However, the introduction of larger molecules has been a recurring problem. It is now agreed that for indigo, the molecules are located on the external surface and at the ends of the fibres, thus blocking access to internal tunnels. We claim, however, that it is possible for indigo molecules to access the internal channels of sepiolite. FTIR and XRD analyses have provided evidence for folding of the sepiolite structure preheated at high temperature (above 350 °C). By comparison, we have shown that for indigo/sepiolite mixtures treated in the same conditions, no change in the crystalline structure of the sepiolite is observed, and that blue samples, related to Maya blue, with indigo molecules incorporated deeply enough into sepiolite to prevent folding of the tunnels, can be obtained. NMR, FTIR and thermal analysis confirm the interaction of indigo with the water coordinated to magnesium(II) and located inside the internal and external channels of sepiolite. Two other hypotheses are excluded; we show both that zeolitic water is not blocked in the tunnels by indigo, and that if thermal decomposition products of indigo can be formed, they are in a minority. 相似文献
10.
Bianco A Furrer J Limal D Guichard G Elbayed K Raya J Piotto M Briand JP 《Journal of combinatorial chemistry》2000,2(6):681-690
The solid-phase synthesis of 2,5-diketopiperazines containing the trans-4-hydroxy-L-proline amino acid residue (Hyp) was performed on Ellman polystyrene, polyoxyethylene-polyoxypropylene (POEPOP), polystyrene-polyoxyethylene NovaSyn, and Wang resins, respectively. The reaction pathway allowed the introduction of different functional groups around the bicyclic scaffold in a combinatorial approach, and it generated mixtures of isomers. A detailed characterization of the single reaction steps by high resolution magic angle spinning (HRMAS) NMR spectroscopy was performed. The NMR spectral resolution of the resin-bound intermediates and final products was greatly influenced by the polymer matrix. The POEPOP resin permitted to obtain HRMAS NMR spectra with a resolution comparable with that of the spectra of the molecules in solution. Moreover, configurational and conformational isomers formed during the solid-phase reaction steps could be detected and easily assigned. Therefore, the combination of the HRMAS NMR technique with the use of nonaromatic resins may become an extremely powerful tool in solid-phase organic synthesis. This approach will allow the monitoring of multistep reactions and the conception of on-bead structural studies either on small molecules or on natural and/or synthetic oligomers. 相似文献