Search results for "Spectroscopy"
showing 10 items of 10293 documents
Darstellung einiger oligomerer Cyclo{oligo[(2-hydroxy-1,3-phenylen)methylen]}e. Spektroskopische Untersuchung ihrer Pseudorotation
1978
Es wird die Darstellung von Cyclo{tris[(2-hydroxy-5-methyl-1,3-phenylen)methylen]-(2-hydroxy-5-tert-butyl-1,3-phenylen)methylen} (4a), Cyclo{bis[(2-hydroxy-5-methyl-1,3-phenylen)methylen]-bis[(2-hydroxy-5-tert-butyl-1,3-phenylen)methylen]}(4b) und Cyclo-{pentakis[(2-hydroxy-5-methyl-1,3-phenylen)methylen]} (4c) beschrieben. Die IR-Spektren zeigen, das die phenolischen Hydroxygruppen der Vierringverbindungen 4a und 4b intramolekulare, vom Losungs(CCl4)- oder Zerteilungsmittel (KBr) weitgehend unabhangige Wasserstoffbrucken bilden, die bei der pentameren Ringverbindung 4c schwacher sind. Anhand der 1H-NMR-Spektren last sich bei diesen Verbindungen eine Pseudorotation nachweisen. Die Massenspe…
Stable adducts of nerve agents sarin, soman and cyclosarin with TRIS, TES and related buffer compounds—Characterization by LC-ESI-MS/MS and NMR and i…
2009
Abstract Buffering compounds like TRIS are frequently used in chemical, biochemical and biomedical applications to control pH in solution. One of the prerequisites of a buffer compound, in addition to sufficient buffering capacity and pH stability over time, is its non-reactivity with other constituents of the solution. This is especially important in the field of analytical chemistry where analytes are to be determined quantitatively. Investigating the enzymatic hydrolysis of G-type nerve agents sarin, soman and cyclosarin in buffered solution we have identified stable buffer adducts of TRIS, TES and other buffer compounds with the nerve agents. We identified the molecular structure of the…
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.
Bis-, Tris-, and Tetrakis(squaraines) Linked by Stilbenoid Scaffolds
2001
The oligosquaraines 1−5, with stilbenoid scaffolds, were prepared by multistep syntheses in which the final steps consisted of condensation reactions between the semisquaric acid 21 and multiple resorcinols 12b−15b and 17b. The target compounds exhibit intense (ϵ > 250000 L·mol−1·cm−1) and sharp absorption bands with maxima between 687 to 778 nm, depending on the conjugation in the stilbenoid scaffold. Comparison with the monosquaraine 6 as a model compound reveals intramolecular interactions between different donor−acceptor−donor moieties, which give rise to increased absorption intensities.
The preparation of (14C) and [3H] labelled benzene oxide
1977
Benzene oxide -[U-14C] was prepared from benzene -(U-14C) by modifications of methods described for the inactive compound. Benzene oxide-[3.6–3H] was prepared by decomposition of 3.6-bis-trimethylsilyl-1,4-cyclohexadiene with tritiated water. bromination of the 1,4-cyclohexadiene-[3,6-3H] so obtained. epoxidation and dehydrobromination. With the latter method benzene oxide-[3,6–3H] can be prepared at a much lower cost and higher specific activity than benzene oxide-[U-14C].
Radioactively labelled epoxides. Part IV. Tritium labelled α- and β-methyl styrene oxides
1983
Tritium labelled α-methyl styrene oxide (2-methyl-2-phenyloxirane) and cis- and trans-β-methyl styrene oxides (Z- and E-2-methyl-3-phenyl oxirane) have been prepared using tritiated water as the inexpensive source of tritium. The two geometrical isomers of β-methyl styrene oxide were synthesized by a sequence of reactions which led to stereochemically pure products, and obviated any need to separate the isomers.
UV-induced solvent free synthesis of truxillic acid–bile acid conjugates
2009
The solvent free UV-induced [2 + 2] intermolecular cycloaddition of two molecules of 3α-cinnamic acid ester of methyl lithocholate produced in 99% yield of α- and e-truxillic acid-bis(methyl lithocholate) isomers, which possess two structurally different potential binding sites. A prerequisite for this effective solid state reaction is a proper self-assembled crystal structure of the starting conjugate crystallized from acetonitrile. The crystallization of cinnamic acid ester of methyl lithocholate from acetonitrile produces two different crystalline forms (polymorphs), which is the reason for the solid state formation of two isomers of truxillic acid-bis(methyl lithocholate).
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…