Search results for "NMR spectra"

1H and 13C NMR Measurements of Dimethylchloroformiminium Chloride and Dimethylformamide Hydrochloride

1979

Dual proton and carbon-13 NMR spectra of dimethylchloroformiminium chloride 1 and dimethylformamide hydrochloride 2 in CDCl3 at different temperatures have been measured and the results compared to proton NMR data of dimethyl formamide 3. The energy barriers of internal rotation about C-N bond in 1 and 2 were considerably lower than that of 3. The values of E were 39.3 for 1, 55.9 for 2 and (lit. value) 89.3 for 3 (in kJ/mole).

Solvent effects of pyridine on the NMR spectra of carboxylic acids. I—study of the acrylic,trans-crotonic and 3-butenoic acids

1975

Proton magnetic resonance spectral parameters of acrylic, trans-crotonic and 3-butenoic acids, their methyl esters and the corresponding alcohols (COOH substituted by CH2OH) have been measured for 5% (w/v) solutions in carbon tetrachloride and in pyridine-d5 at 33·5 °C. The total solvent effect of pyridine on the shifts of the skeleton protons of the acid was found to consist of three different effects independently measured from the reference samples.

High-pressure NMR spectroscopy: An in situ tool to study tin-catalyzed synthesis of organic carbonates from carbon dioxide and alcohols. Part 2 [1]

2015

Dialkoxide diorganotin(IV) complexes are known to readily react with carbon dioxide under pressure and they are considered as suitable catalyst precursor models for the direct synthesis of organic carbonates. To gain a better understanding of CO2 insertion processes with Sn-OR bonds, the reactivity of n-Bu2Sn(OCH(CH3)(2))(2) (2) was investigated using high-pressure NMR (HP-NMR) spectroscopy. In deuterated solvents (isopropanol-d(8) and toluene-d(8)) under 50 bar of CO2 pressure at 80 degrees C, Sn-119{H-1} NMR experiments revealed the exclusive formation of an unprecedented tetraorganodistannoxane species, characterized as the bis[diisopropycarbonatotetrabutyldistannoxane] complex, {[n-Bu2S…

Substituted methyl 5β-cholan-24-oates. I—17O NMR spectral characterization

1994

Methyl esters of four common bile acids, 3α-hydroxy-5-β-cholan-24-oic (lithocholic) acid, 3α, 7α-dihydroxy-5β-cholan-24-oic (chenodeoxycholic) acid, 3α,12α-dihydroxy-5β-cholan-24-oic (deoxycholic) acid and 3α,7α,12α-trihydroxy-5β-cholan-24-oic (cholic) acid, and 14 acetylated, trifluoroacetylated, mesylated and oxo derivatives of methyl 5β-cholan-24-oates were prepared and their 17O NMR spectra recorded. In spite of their relatively high molecular masses and the rigid molecular structure of the steroid skeleton, most of the oxygens included in these structures gave well resolved 17O NMR resonance lines at natural abundance in 0.25–0.5 M acetonitrile solutions at 75°C. In agreement with the …

Crystal structure transformations induced by surface stresses in BaTiO3and BaTiO3@SiO2nanoparticles and ceramics

2015

International audience; Lattice structure transformations in nanopowders of ferroelectric BaTiO3 and BaTiO3@SiO2 core-shell nanostructured ceramics were studied by nuclear magnetic resonance (NMR) and electron paramagnetic resonance (EPR) at the temperatures 120–450 K and particle size of 300 and 500 nm. NMR spectra of all studied samples in the paraelectric phase are identical to the spectra in bulk material indicating their perfect perovskite structure without visible influence of particle surface. However, we have found that surface of particles essentially influence the ferroelectric phase transitions detected by both NMR and EPR techniques. The strongest changes as compared to bulk mat…

Book Review: One Dimensional and Two Dimensional NMR Spectra by Modern Pulse Techniques. Edited by K. Nakanishi

1992

Synthesis, spectroscopic (Mössbauer, IR and NMR) and X-ray structural studies of diorganotin complexes of 2,2′-bipyrimidine and further NMR studies o…

1996

Abstract The ligand 2,2′-bipyrimidine (bipym) was reacted with diorganotins R 2 SnCl 2 (R = methyl, ethyl) and complexes of the types R 2 SnCl 2 bipym, R 2 SnCl 2 bipym · bipym and (R 2 SnCl 2 ) 2 bipym were synthesized and studied by 1 H and 13 C NMR spectroscopy in solution, and by IR and Mossbauer spectroscopy in the solid state and frozen solutions. The complexes Et 2 SnCl 2 bipym · bipym and (Et 2 SnCl 2 ) 2 bipym were characterized by X-ray diffraction methods. In both complexes the tin environment is octahedral with chloro atoms in a cis disposition, the ethyl groups in a trans disposition and two N atoms from the ligand bipym. the second complex is a centrosymmetric binuclear specie…

Secondary interactions as driving force in heterocomplex formation of 2,7-disubstituted-1,8-naphthyridines: Quantum chemical, NMR and mass spectral i…

2009

Abstract Tautomerism and dimerization of 2,7-disubstituted-1,8-naphtyridines has been studied theoretically by quantum chemical methods and experimentally by liquid and solid state NMR and ESI-TOF mass spectral techniques. The heterocomplex formation has been proven in solution by variable temperature 1H NMR and in solid state by 13C CPMAS NMR spectra of a grinded mixture of two congeners. Secondary interactions have been proposed as driving forces in the heterocomplex formation. The energy differences between homo- and heterocomplexes were calculated with recently developed DFT + D methods. The energy data obtained by the quantum chemical methods are in agreement with the concept of second…

DFT and experimental studies on structure and spectroscopic parameters of 3,6-diiodo-9-ethyl-9H-carbazole

2015

The first report on crystal and molecular structure of 3,6-diiodo-9-ethyl-9H-carbazole is presented. Experimental room-temperature X-ray and 13C chemical shift studies were supported by advanced theoretical calculations using density functional theory (DFT). The 13C nuclear magnetic shieldings were predicted at the non-relativistic and relativistic level of theory using the zeroth-order regular approximation (ZORA). Theoretical relativistic calculations of chemical shifts of carbons C3 and C6, directly bonded to iodine atoms, produced a reasonable agreement with experiment (initial deviation from experiment of 44.3 dropped to 4.25 ppm). The changes in ring aromatic character via simple harm…

Molecular modeling and experimental studies on structure and NMR parameters of 9-benzyl-3,6-diiodo-9H-carbazole

2015

A combined experimental and theoretical study has been performed on 9-benzyl-3,6-diiodo-9H-carbazole. Experimental X-ray (100.0 K) and room-temperature 13C NMR studies were supported by advanced density functional theory (DFT) calculations. The non relativistic structure optimization was performed and the 13C nuclear magnetic shieldings were predicted at the relativistic level of theory using the Zeroth Order Regular Approximation (ZORA). The changes in the benzene and pyrrole rings compared to the unsubstituted carbazole or the parent molecules were discussed in terms of aromaticity changes using the harmonic oscillator model of aromaticity (HOMA) and the nucleus independent chemical shift…