Synthesis, structure and characterisation of late transition metal complexes with 2-(tetrazol-1-yl)pyridine

Characterization of lignin by 1H and 13C NMR spectroscopy

Nonplatinum metal complexes of [Pd(L1)Cl2] (C1), [Rh(L1)Cl3(DMSO)] (C2), [Pd(L2)Cl2] (C3), and [Rh(L3)Cl3(DMSO)] (C4) with isoquinoline derivatives have been prepared and characterized. C1–C4 exhib...

The synthesis of hypotaurine and taurine was investigated in astroglia-rich primary cultures obtained from brains of neonatal Wistar rats using 1H and 13C nuclear magnetic resonance (NMR) spectroscopy. Cell extracts of astroglial cultures analyzed by 1H NMR spectroscopy show prominent signals of hypotaurine. To identify cysteine as precursor for hypotaurine and taurine synthesis in astroglial cells, primary cultures were incubated with [3-(13)C]cysteine for 24 or 72 h. Cell extracts and incubation media were then analyzed with 13C NMR spectroscopy. Labeled hypotaurine, taurine, glutathione, and lactate were identified in the cell extracts. Within 72 h, 35.0% of the total intracellular hypotaurine and 22.5% of taurine were newly synthesized from [3-(13)C] cysteine. The presence of [1-(13)C]hypotaurine and [1-(13)C]taurine in the incubation medium proves the release of those products of cysteine metabolism into the medium. Minor amounts of the [3-(13)C]cysteine were used for the synthesis of glutathione in astroglial cells or metabolized to [3-(13)C]lactate, which was found in cell extracts and media. These results indicate that the formation of hypotaurine and taurine is a major pathway of cysteine metabolism in astroglial cells.

Background: Tuberculosis (TB), a disease caused by the bacillus bacteria Mycobacterium tuberculosis is one of the major contributors of ill health in the world. TB is ranked in the top 10 causes of death globally and it is the leading killer associated with a single infectious agent. According to the World Health Organization (WHO), global number of deaths associated with TB have been slowly declining with 1.3 million in reported 2016 and 2017, and 1.2 million reported in 2018 and 2019. Objective: The synthesis, characterisation, biological evaluations, and the prediction of ADMET properties of the novel benzylamine derivatives. Methods: Commercially available reagents and solvents were purchased from Sigma Aldrich and Merck (South Africa). All chemicals were used as received, unless otherwise stated. The synthesised crude compounds were purified by flash silica gel column chromatography (5 – 30% ethyl acetate in hexane). The successful formation and purity of the synthesised compounds was confirmed by NMR, HRMS and melting point. Results: The respective organic compounds were synthesised by treating 3-ethoxysalcyladehyde, 5-bromo-3-ethoxysalcyladehyde, 5-chloro-3-ethoxysalcyladehyde with various aromatic amines and the products were obtained in good to excellent yields. The 1H and 13C NMR spectra of all the products showed the appearance of the methylene signals ranging from 3.88 – 4.68 ppm and 42.25 – 52.57 ppm respectively. Additionally, most compounds showed anti-Mycobacterium tuberculosis activity that ranged between 20 and 28 µM. Conclusion: A total of 36 compounds were synthesised and successfully biologically evaluated against Mycobacterium tuberculosis (Mtb) H37RV strain. All compounds showed activity against Mtb at concentrations of > 20 µM < 28 µM with the exception of compound one that was active against Mtb at higher concentration (MIC90 > 125 µM).

The molecular composition of heavy oil and bitumen is critical for process design calculations and for the selection of production and refining processes, reaction schemes, and conditions that optimize their economic value. These materials remain ill-defined on a molecular basis. For example, diverse molecular structures have been proposed for asphaltenes on the basis of the same physical samples and analytical data [1H and 13C nuclear magnetic resonance (NMR) spectroscopy, mass spectroscopy, and elemental composition]. Molecule construction algorithms appear under constrained by these analytical data, particularly at the molecular subunit length scale (e.g., naphthenic and aromatic groups and aliphatic chains) from both an identification and a mass balance perspective. In this work, we address whether spectral data can provide additional constraints at this length scale that reduces the ambiguity of outcomes from molecule construction algorithms, by making use of spectral data for possible subunits. In this proof of concept investigation, infrared (IR), Raman, and 1H and 13C NMR spectra were computed using density functional theory (DFT) and the B3LYP/6-311G basis set. The molecular subunits present in more than 20 large molecules were probed by spectral subtraction based on spectral contributions from a library of small molecules, because it is at this length scale that the greatest uncertainty in molecule identification and construction algorithms appears to arise. Spectral subtraction using 1H NMR spectroscopy failed to identify molecular subunits in any of the more than 20 large molecules evaluated. 13C NMR spectroscopy identified only 3 large molecules. In contrast, joint use of IR and Raman spectroscopy identified more than 75% of the aromatic subunits present, and naphthenic and aromatic subunits were discriminated. Aliphatic chain length remained poorly defined, and the resulting molecule compositions are qualitative. It is expected that the results of this work will inform molecule construction and identification algorithms for ill-defined hydrocarbons.

Adducts of rhodium(II) tetraacylates with methionine and its derivatives: 1H and 13C nuclear magnetic resonance spectroscopy and chiral recognition

Characterization of oligo(acrylic acid)s and their block co-oligomers

Infra-red (IR) spectroscopy, conductimetric titration, 1H and 13C nuclear magnetic resonance (NMR) spectroscopies have been assessed for their reliability in determining the composition of polymers obtained by hydrocar-boxylation of polybutadienes. 1H NMR data can be successfully applied to the analysis of polymers that have been selectively hydrocarboxylated on only the terminal C atoms of the pendant double bonds or of polymers that have phenyl end groups. For polymers that have H, OH or CO2H termination and which have been hydrocarboxylated in a non-selective manner, it is necessary to use a combination of 1H and 13C NMR spectroscopies with due allowance being made for the different receptivities of different kinds of carbon atoms. Conductimetric titrations give information on the overall conversion of double bonds to carboxylic acids but not on the detailed microstructure of the polymer. Problems are encountered in some cases because of precipitation of the polymer during the titration as a partial sodium salt. IR spectroscopy is not suitable for analysis of these polymers because of large background absorption in the appropriate region.

Aphanizomenon flos-aquae (AFA) cyanobacteria from Klamath Lake (Oregon) are considered a "superfood" due to their broad nutritional profile that has proved to have health-enhancing properties. The AFA metabolome is quite complex. Here, we present a study that, combining multinuclear 1H, 31P, and 13C Nuclear Magnetic Resonance (NMR) spectroscopy and high-resolution mass spectrometry, led to the detection of uncommon phosphorylated metabolites in AFA. We focused our attention on 31P NMR signals at 20 ppm, a chemical shift that usually points to the presence of phosphonates. The molecules contributing to 20 ppm 31P NMR signals revealed, instead, to be nucleoside 2',3'-cyclic monophosphates. These metabolites were fully characterized by multinuclear 1H, 31P, and 13C NMR spectroscopy and high-resolution mass spectrometry.

Bacterial strain XII, which belongs to the family Pseudomonad, utilizes 1-chloro-4-nitrobenzene as a sole source of carbon, nitrogen, and energy. Suspensions of 1-chloro-4-nitrobenzene -grown cells removed 1-chloro-4-nitrobenzene from culture fluids, and there was a concomitant release of ammonia and chloride. Under anaerobic conditions XII transformed 1-chloro-4-nitrobenzene into a product which was identified as 2-amino-5-chlorophenol by 1H and 13C nuclear magnetic resonance (NMR) spectroscopy and mass spectrometry. This transformation indicated that there was partial reduction of the nitro group to the hydroxylamino substituent, followed by Bamberger rearrangement. In the presence of oxygen but in the absence of NAD, fast transformation of 2-amino-5-chlorophenol into a transiently stable yellow product was observed with resting cells and cell extracts. This compound exhibited an absorption maximum at 395 nm and was further converted to a dead-end product with maxima at 226 and 272 nm. The compound formed was subsequently identified by 1H and 13C NMR spectroscopy and mass spectrometry as 5-chloropicolinic acid. In contrast, when NAD was added in the presence of oxygen, only minor amounts of 5-chloropicolinic acid were formed, and a new product, which exhibited an absorption maximum at 306 nm, accumulated.

Complexation of selenomethionine and its derivatives with some dimeric rhodium(II) tetracarboxylates: 1H and 13C nuclear magnetic resonance spectroscopy

Chapter Two - 1H and 13C Nuclear Magnetic Resonance Spectroscopy

Characterization of macroaggregates and photodegradation of their water soluble fraction

Extraction of multiple pure component 1H and 13C NMR spectra from two mixtures: Novel solution obtained by sparse component analysis-based blind decomposition

Preparation, characterization and photochemistry of 4,4′-diacetamidostilbene and its β-cyclodextrin inclusion complex