Search results for "Nuclear magnetic resonance"
showing 10 items of 1743 documents
Comparison of transflection and transmission FTIR imaging measurements performed on differentially fixed tissue sections
2015
The widespread and cost-effective use of transflection substrates in Fourier transform infrared (FTIR) imaging of clinical samples is affected by the presence of artefacts including the electric field standing wave (EFSW) and contributions from light dispersion. For IR-based diagnostics, the manifestation of undesirable artifacts can distort the spectra and lead to erroneous diagnosis. Nevertheless, there is no clear consensus in the literature about the degree of influence of these effects. The aim of this work is to contribute to this discussion by comparing transflection and transmission images of the same tissue. For this purpose two adjacent sections of the same tissue (lymphoma sample…
Titanium Complexes Stabilized by a Sulfur‐Bridged Chelating Bis(aryloxo) Ligand as Active Catalysts for Olefin Polymerization
2004
The mixed-ligand complexes [Ti2(μ-OR)2(OR)2(κ3-tbop)2] (1a) for R = Me and (1b) R = Et were prepared by the reaction of Ti(OR)4 and H2tbop {H2tbop = 2,2′-thiobis[4-(1,1,3,3-tetramethylbutyl)phenol]} in methanol. Treatment of 1a and 1b with AlMe3 led to the substitution of terminal alkoxy groups to create the organometallic compounds [Ti2(μ-OR)2(κ3-tbop)2(Me)2] (2a) for R = Me and (2b) for R = Et. Controlled hydrolysis of 2b causes the evolution of methane and the formation of the titanoxane compounds [{Ti2(μ-OEt)2(κ3-tbop)2}2(μ-O)2]·2CH2Cl2 (3). Structures of 1a, 1b, 2a, 2b, and 3 were confirmed by NMR spectroscopy; 1b and 3 were further investigated with X-ray crystallography. Compounds 1a…
Titanium Complexes of Chelating, Dianionic O,S,O‐Bisphenolato Ligands: Syntheses, Characterisation, and Catalytic Activity
2005
Titanium complexes based on 2,2'-thiobis[4-(1,1,3,3-tetramethylbutyl)phenolato] (tbop) are prepared by reaction of TiCl 4 or Ti(NMe 2 ) 4 with the parent biphenol. Three new complexes are reported: [Ti 2 (μ-tbop-κ 3 O,S,O)(μ-tbop-κ 2 O,O)-(tbop-κ 3 O,S,O)Cl 2 ] (1).2CH 3 CN, [Ti 2 (μ-tbop-κ 3 O,S,O) 2 Cl 4 ] (2) and [Ti(tbop-κ 3 O,S,O) 2 ] (3). Substitution of the chlorides in 1 and 2 by 2,6-diisopropylphenolato and imido (NtBu) ligands generates the new compounds [Ti 2 (μ-tbop-κ 3 O,S,O) 2 -Cl 2 (dipp) 2 ] (4).Et 2 O and [Ti 2 (μ-tbop-κ 3 O,S,O) 2 (NtBu) 2 -(NH 2 tBu) 2 ] (5), respectively. Treatment of 5 with crude Me 3 -SiCl, containing Me 3 SiOH, produces [Ti(tbop-κ 3 O,S,O)Cl(O-SiMe 3 …
Cytotoxic neo-clerodane diterpenes from Stachys aegyptiaca
2018
Abstract Two new E/Z neo-clerodane diterpene isomers, trivially named stachaegyptin D (1) and E (2), together with known compounds, stachysolon monoacetate (3) and stachysolon diacetate (4), were isolated from an organic-solvent extract of the medicinal herb Stachys aegyptiaca. Structures were elucidated by a combination of spectroscopic methods, including HREIMS, 1H, 13C, DEPT, and 2D NMR analysis, as well as, first time X-ray analysis for stachysolone (3). All isolated metabolites showed some activity against the human hepatocellular cell line, HepG2. Compound 4 was the most active with an IC50 of 59.5 μM.
Synthesis of the Glycopeptide Partial Sequence A80-A84 of Human Fibroblast Interferon
1985
The glycopentapeptide H-(GlcNAcβ1-)Asn-Glu-Thr-Ile-Val-OH (10) representing the partial sequence A80–A84 of human fibroblast interferon was synthesized using the newly developed allyl-ester protection of carboxy functions. The allyl esters, which are stable to acids and to bases, can be cleaved under very mild, neutral conditions using tris(triphenylphosphine)rhodium(I) chloride or tetrakis(triphenylphosphine)palladium(0) as a catalyst. This synthetic method opens up a preparative route to glycopeptide model structures of glycoproteins of high biological interest.
Tris(2-thienyl)methyl cation; An unprecedent 13C NMR behavior
1986
Abstract An unexpected response of the chemical shift value to the substitution of phenyl by thienyl groups is found in the series 1–8 . On this basis the planar cation 7 appears to show an homoaromatic-like peripheral ring current.
Predicting 19F NMR Chemical Shifts: A Combined Computational and Experimental Study of a Trypanosomal Oxidoreductase–Inhibitor Complex
2020
Abstract The absence of fluorine from most biomolecules renders it an excellent probe for NMR spectroscopy to monitor inhibitor–protein interactions. However, predicting the binding mode of a fluorinated ligand from a chemical shift (or vice versa) has been challenging due to the high electron density of the fluorine atom. Nonetheless, reliable 19F chemical‐shift predictions to deduce ligand‐binding modes hold great potential for in silico drug design. Herein, we present a systematic QM/MM study to predict the 19F NMR chemical shifts of a covalently bound fluorinated inhibitor to the essential oxidoreductase tryparedoxin (Tpx) from African trypanosomes, the causative agent of African sleepi…
Antileukemic ancistrobenomine B and related 5,1′-coupled naphthylisoquinoline alkaloids from the Chinese liana Ancistrocladus tectorius
2017
A striking feature of the metabolite pattern of the Southeast Asian liana Ancistrocladus tectorius (Ancistrocladaceae) is the predominance of 5,1′-coupled naphthylisoquinoline alkaloids. About 20 alkaloids of this coupling type have so far been discovered in this plant species. Here, we report on the isolation of four new 5,1′-linked naphthylisoquinolines from the twigs and stems of A. tectorius. Two of them, the ancistrobenomines B (5) and C (6), belong to the very rare group of alkaloids with a fully dehydrogenated isoquinoline portion. Likewise unusual for naphthylisoquinoline alkaloids is the presence of a hydroxymethylene group at C-3. Within the large class of meanwhile ca. 180 such n…
Inhibitor-Induced Dimerization of an Essential Oxidoreductase from African Trypanosomes
2018
Trypanosomal and leishmanial infections claim tens of thousands of lives each year. The metabolism of these unicellular eukaryotic parasites differs from the human host and their enzymes thus constitute promising drug targets. Tryparedoxin (Tpx) from Trypanosoma brucei is the essential oxidoreductase in the parasite's hydroperoxide-clearance cascade. In vitro and in vivo functional assays show that a small, selective inhibitor efficiently inhibits Tpx. With X-ray crystallography, SAXS, analytical SEC, SEC-MALS, MD simulations, ITC, and NMR spectroscopy, we show how covalent binding of this monofunctional inhibitor leads to Tpx dimerization. Intra- and intermolecular inhibitor-inhibitor, pro…
Antiproliferative activity against leukemia cells of sesquiterpene lactones from the Turkish endemic plant Centaurea drabifolia subsp. detonsa
2017
The apolar organic extract obtained from aerial parts of Centaurea drabifolia Sibth. & Sm. subsp. detonsa (Bornm.) Wagenitz, growing wild in Turkey, was investigated for the first time for its secondary metabolite composition. Seven sesquiterpene lactones belonging to the guaiane class (1-7), including the new compound 4, along with a fatty acid lactone derivative (8), were isolated. The structures of these compounds were established by spectroscopic analysis, including 2D NMR spectroscopic techniques, with the stereostructure of the new guaiane 4 determined with the help of MTPA derivatization. Cytotoxic activities of compounds 1-7 were evaluated against two cancer cell lines, namely acute…