Search results for "1h nmr spectroscopy"
showing 10 items of 23 documents
The synthesis of metallocene-labelled drugs for biological assays
1990
Several drugs (amphetamine, desipramine, nortriptyline, phenobarbital) have been labelled with metallocenic fragments in order to develop a new immunoassay method. The metallocenic fragments are cymantrenic or benchrotrenic derivatives: the linkage between the organic and organometallic moieties has been achieved by reactions between amino and acidic functional groups. All the products (metallohaptens), purified by different chromatography techniques, have been fully characterized by IR and 1H NMR spectroscopy and their mass spectra.
First synthesis of single-“strapped cyclam-porphyrins”
1994
The first synthesis of strapped cyclam porphyrins is described ; these will be studied as dioxygen carriers as well as cytochrome C oxidase models. The original derivatives are characterized by mass spectrometry and 1H NMR spectroscopy. The cofacial conformation of the two different macrocycles is confirmed by 1H NMR data.
Application of 1H NMR-based serum metabolomic studies for monitoring female patients with rheumatoid arthritis
2015
AbstractRheumatoid arthritis is a chronic autoimmune-based inflammatory disease that leads to progressive joint degeneration, disability, and an increased risk of cardiovascular complications, which is the main cause of mortality in this population of patients. Although several biomarkers are routinely used in the management of rheumatoid arthritis, there is a high demand for novel biomarkers to further improve the early diagnosis of rheumatoid arthritis, stratification of patients, and the prediction of a better response to a specific therapy.In this study, the metabolomics approach was used to provide relevant biomarkers to improve diagnostic accuracy, define prognosis and predict and mon…
Aromatic Bridged Bis-phenol A Derived Cyclophanes. Synthesis, Molecular Structure and Binding Properties Toward Quats
2003
Three novel polyoxyethylene bridged bis phenol A derived cyclophanes, {\rm 2 -- 4,} with additional aromatic units in the bridge to increase the number of cation–π interactions with guest cations, were synthesized and characterized by means of X-ray crystal structure determinations. The binding properties of these receptors toward tetramethylammonium (TMA), N-methylpyridinium (NMP), acetylcholine (ACh) and N-methylquinolinium (NMQ) salts were evaluated by means of 1H NMR spectroscopy and compared with those of the previously reported receptor 1.
Chemometrics as a Tool of Origin Determination of Polish Monofloral and Multifloral Honeys
2014
The aim of this study was to evaluate the application of chemometrics studies to determine the botanical origin of Polish monofloral honeys using NMR spectroscopy. Aqueous extracts of six kinds of honeys, namely, heather (Calluna vulgaris L.), buckwheat (Fagopyrum esculentum L), lime (Tilia L), rape (Brassica napus L. var. napus), acacia (Acacia Mill.), and multifloral ones, were analyzed. Multivariate chemometric data analysis was performed using principal component analysis (PCA) and orthogonal partial least-squares discriminant analysis (OPLS-DA). Chemometric analysis supported by pollen analysis revealed the incorrect classification of acacia honeys by the producers. Characteristic moti…
N-(2,3,5,6-Tetrafluoropyridyl)sulfoximines: synthesis, X-ray crystallography, and halogen bonding
2020
In the presence of KOH, NH-sulfoximines react with pentafluoropyridine to give N-(tetrafluoropyridyl)sulfoximines (NTFP-sulfoximines) in moderate to excellent yields. Either a solution-based or a superior solvent-free mechanochemical protocol can be followed. X-Ray diffraction analyses of 26 products provided insight into the bond parameters and conformational rigidity of the molecular scaffold. In solid-state structures, sulfoximines with halo substituents on the S-bound arene are intermolecularly linked by C–X⋯OS (X = Cl, Br) halogen bonds. Hirshfeld surface analysis is used to assess the type of non-covalent contacts present in molecules. For mixtures of three different S-pyridyl-substit…
Substituted Dibenzothiophenes I: Synthesis, Chromatography, Mass Spectrometry and Structure Elucidation by1H NMR Spectroscopy
1992
Abstract Some polychlorinated and polymethylated dibenzothiophenes have been synthesized to serve as model compounds in environmental analysis. In order to obtain pure isomers, the synthesis mixtures have been fractionated with reversed-phase high performance liquid chromatography. In spite of a high sensitivity, mass spectrometry does not provide any reliable way to determine the precise structures of different isomers. Therefore, 1H NMR spectroscopy has been utilized as an aid in their analysis. The structures for two isomeric tetramethyldibenzothiophenes could be suggested on the basis of their 1H NMR spectra. Also some proposals for possible structures of two isomeric trimethyldibenzoth…
On the Ion-Pair Recognition and Indication Features of a Fluorescent Heteroditopic Host Based on a BODIPY Core
2014
A fluorescent heteroditopic host for ion pairs and zwitterionic species has been synthesized. Its affinity towards a series of anions, cations and ion pairs in acetonitrile has been assessed, and the spectroscopic response has been evaluated. Solid–liquid extraction experiments of inorganic salts, α-amino acids and γ-aminobutyric acid (GABA) into acetonitrile solutions were performed, and the resulting complexes were analyzed by UV/Vis absorption, fluorescence and 1H NMR spectroscopy. The discrimination patterns observed have been rationalized in terms of the molecular topologies of the host and guests.
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.
Reversible complexation of ethylene by a silylene under ambient conditions.
2014
Treatment of toluene solutions of the silylenes Si(SArMe6)2 (ArMe6 = C6H3-2,6(C6H2-2,4,6-Me3)2, 1) or Si(SArPri4)2 (ArPri4 = C6H3-2,6(C6H3-2,6-Pri2)2, 2) with excess ethylene gas affords the siliranes (ArMe6S)2tiebar above startSiCH2tiebar above endCH2 (3) or (ArPri4S)2tiebar above startSiCH2tiebar above endCH2 (4). Silirane 4 evolves ethylene spontaneously at room temperature in toluene solution. A Van’t Hoff analysis by variable-temperature 1H NMR spectroscopy showed that ΔGassn = −24.9(2.5) kJ mol–1 for 4. A computational study of the reaction mechanism using a model silylene Si(SPh)2 (Ph = C6H5) was in harmony with the Van’t Hoff analysis, yielding ΔGassn = −24 kJ mol–1 and an activatio…