Search results for "nmr spectroscopy"
showing 10 items of 119 documents
Five-to-Six Membered Ring-rearrangements in the Reaction of 5-Perfluoroalkyl-1,2,4-oxadiazoles with Hydrazine and Methylhydrazine
2006
The hydrazinolysis reaction of 5-perfluoroalkyl-1,2,4-oxadiazoles with hydrazine or methylhydrazine as bidentate nucleophiles has been investigated. The reaction occurred through the addition of the bidentate nucleophile to the C(5)-N(4) double bond of the 1,2,4-oxadiazole followed by ring-opening and ring-closure (ANRORC) involving the second nucleophilic site of the reagent. This ring-closure step could involve either the original C(3) of the 1,2,4-oxadiazole (giving a five-to-five membered ring rearrangement) or an additional electrophilic center linked to it (exploiting a five-to-six membered ring rearrangement). An alternative initial nucleophilic attack may involve the additional elec…
Binding and Fluorescent Sensing of Dicarboxylates by a Bis(calix[4]pyrrole)-Substituted BODIPY Dye
2013
A bis(calix[4]pyrrole)-substituted BODIPY ditopic receptor 1 has been synthesised and characterised. The binding and sensing properties of 1 towards several aliphatic and aromatic dicarboxylates have been evaluated by using UV/Vis fluorescence and 1H NMR spectroscopy. The receptor strongly binds linear α,ω-dicarboxylates of appropriate lengths (C9 and C10) by acting as a cleft. For all dicarboxylates, the binding event is detected by a bathochromic shift in the UV/Vis spectra of the receptor and by strong quenching of its fluorescence.
On the mechanistic behavior of highly efficient palladium-tetraphosphine catalytic systems for cross-coupling reactions: first spectroscopic and elec…
2008
Electrochemical studies carried out in conjunction with 31P NMR spectroscopy on the palladium(II)/palladium(0) halogeno complexes of the tetraphosphine 1,1′,2,2′-tetrakis(diphenylphosphino)-4,4′-di...
Synthesis of Both Ionic Species of Ammonium Dithiocarbamate Derived Cholic Acid Moieties
2011
The reaction of 3-aminopropylamide of cholic acid with CS₂ produced a bile acid derivative of dithiocarbamic acid which further formed an ammonium salt with another molecule of 3-aminopropylamide of cholic acid. The cationic 3-ammonium propylamide of cholic acid did not react further with CS₂ and the formed salt was stable in the reaction mixture, even when excess CS₂ was used. When the reaction was carried out in the presence of aqueous sodium hydroxide, only the bile acid derivative of sodium dithiocarbamate was formed. The dithiocarbamate derivatives were characterized by ¹H- and ¹³C-NMR spectroscopy and ESI-TOF mass spectrometry. peerReviewed
1H, 13C and 15N NMR chemical shift assignments of cAMP-regulated phosphoprotein-19 and -16 (ARPP-19 and ARPP-16)
2020
Protein Phosphatase 2A, PP2A, the principal Serine/threonine phosphatase, has major roles in broad range of signaling pathways that include regulation of cell cycle, cell proliferation and neuronal signaling. The loss of function of PP2A is linked with many human diseases, like cancer and neurodegenerative disorders. Protein phosphatase 2A (PP2A) functions as tumor suppressor and its tumor suppressor activity is inhibited by the overexpression of PP2A inhibitor proteins in most of the cancers. ARPP-19/ARPP-16 has been identified as one of the potential PP2A inhibitor proteins. Here, we report the resonance assignment of backbone 1H, 13C and 15N atoms of human ARPP-19 and ARPP-16 proteins. T…
Synthesis and characterization of a novel high luminescent gold-2-mercapto-1-methyl-imidazole complex
2010
Synthesis and characterization of a new gold-2-mercapto-1-methyl imidazole are reported. This new organic material shows an extraordinary fluorescence activity (superfluorescence) up to 220°C with an unusual quantum yield of 0.2. Both fluorescence and NMR spectroscopy were applied to understand the behavior of the gold-2-mercapto-1-methylimidazole complex. Results suggest that the superfluorescence activity can be attributed to the shrinking of the HOMO-LUMO band gap energy following complexation of the organic imidazole system with gold. Copyright © 2010 John Wiley & Sons, Ltd.
Host-Guest Interactions of Sodiumsulfonatomethyleneresorcinarene and Quaternary Ammonium Halides : An Experimental-Computational Analysis of the Gues…
2020
The molecular recognition of nine quaternary alkyl- and aryl-ammonium halides (Bn) by two different receptors, Calkyl-tetrasodiumsulfonatomethyleneresorcinarene (An), were studied in solution using 1H NMR spectroscopy. Substitution of methylenesulfonate groups at 2-positions of resorcinol units resulted in an increase of cavity depth by ∼2.80 Å and a narrow cavity aperture compared to Calkyl-2-H-resorcinarenes. The effect of alkyl chain lengths on the endo-complexation, that is the ability to incorporate other than N-methyl chains inside the cavities, were investigated using ammonium cations of the type ⁺NH2(R1)(R2), (R1 = Me, Et, Bu, R2 = Bu, Ph, Bz ). The C−H⋯ interactions between guests …
Geminal Ionic Liquids: A Combined Approach to Investigate their Tridimensional Structure
2009
Different investigations, such as 1D and 2D NMR spectroscopy, resonance light scattering spectroscopy and molecular dynamics simulations, have been jointly used to achieve a deeper understanding of the degree of structural order in two geminal ionic liquids. In particular, 3,3’-di-n-butyl-1,1’-(1,3- phenylenedimethylene)diimidazolium and 3,3’-di-n-butyl-1,1’-(1,4-phenylenedimethylene) diimidazolium bis- ACHTUNGTRENUNG[bis(trifluoromethanesulfonyl)imide] have been studied. These geminal ionic liquids were chosen because of the presence of both a rigid phenylenedimethylene link between two imidazolium rings, which should give a high degree of order to the solvent system, and the different sha…
Anion Responsive Molecular Switch Based on a Doubly‐Strapped Calix[4]pyrrole
2022
A calix[4]pyrrole receptor bearing two proximally meso - meso linking isophthaloyl straps displays open and closed states depending on the calix[4]pyrrole conformation. In the crystal structures and in non-polar solvent, the calix[4]pyrrole adopts open 1,3-alternate conformation with straps on the sides. Anion binding triggers a closed state of the receptor providing two types of interactions with an aromatic benzoate guest: hydrogen bonds from the pyrrolic groups and π ··· π interactions from the phenyl groups of the straps. Slow exchange dynamics was observed on the NMR timescale indicating that benzoate, acetate and chloride anions, which bind with relatively low affinity get kinetically…
Direct detection of 17O NMR in [Gd(DOTA)]- by NMR Spectroscopy
2015
The 17O NMR spectrum of the non-coordinated carboxyl oxygen in the GdIII-DOTA (DOTA = tetraazacyclododecanetetraacetic acid) complex has been observed experimentally. Its line width is essentially unaffected by paramagnetic relaxation due to gadolinium, and is only affected by the quadrupole pathway. The results are supported by the relevant parameters (hyperfine and quadrupole coupling constants) calculated by relativistic DFT methods. This finding opens up new avenues for investigating the structure and reactivity of paramagnetic GdIII complexes used as contrast agents in magnetic resonance imaging.