Search results for "Nuclear magnetic resonance spectroscopy"
showing 10 items of 843 documents
2-Acylamino- and 2,4-bis(acylamino)pyrimidines as supramolecular synthons analysed by multiple non-covalent interactions. DFT, X-ray diffraction, and…
2012
Intermolecular interactions of ten 2-acylamino and 2,4-bis(acylamino)pyrimidines (7 of which are previously unknown) have been investigated by X-ray structural, quantum chemical (DFT), and NMR spectral methods. Especially the concentration dependencies of the (1)H NMR chemical shifts and titrations with other molecules capable of multiple hydrogen bonding provided useful information regarding their association via triple or quadruple hydrogen bonding, which is controlled by the conformational preferences of 2-acylamino- and 2,4-bis(acylamino)pyrimidines. On comparison of the properties of 2-acylamino- and 2,4-bis(acylamino)pyrimidines with the corresponding pyridines, an additional nitrogen…
A new oleanane glycoside from the roots ofAstragalus caprinus
2006
A novel oleanane-type triterpene saponin (1) together with two known molecules, soyasapogenol B and astragaloside VIII were isolated from the roots of Astragalus caprinus. Their structural elucidation was performed mainly by 2D NMR techniques (COSY, TOCSY, NOESY, HSQC, HMBC) and mass spectrometry. Compound 1 was determined as 3-O-[alpha-L-rhamnopyranosyl-(1 --> 2)-beta-D-glucuronopyranosyl]-22-O-beta-D-apiofuranosyl-soyasapogenol B.
Normal-phase (temperature gradient) interaction chromatography – A powerful tool for the characterisation of high molecular weight chain-end function…
2015
Abstract We report here, for the first time, quantitative analysis of end-group functionalisation and the extent of end-group modification of polymers with molar mass up to 200,000 g mol −1 , using a combination of isothermal and temperature gradient interaction chromatography. At such high molecular weights, other common analytical techniques such as MALDI-ToF-MS and NMR spectroscopy are simply unable to offer any quantitative insight into the end-group functionality of polymers. Thus, normal phase isothermal interaction chromatography (NP-IIC) has been used to characterise a series of polystyrene samples, with identical molar mass (c. 90,000 g mol −1 ), each carrying a single chain-end fu…
Acylated triterpene saponins from the roots of Securidaca longepedunculata.
2009
Abstract Four triterpene saponins , 3- O -β- d -glucopyranosylpresenegenin 28- O -β- d -apiofuranosyl-(1 → 3)-β- d -xylopyranosyl-(1 → 4)-[β- d -apiofuranosyl-(1 → 3)]-α- l -rhamnopyranosyl-(1 → 2)-{4- O -[( E )-3,4,5-trimethoxycinnamoyl]}-β- d -fucopyranosyl ester, 3- O -β- d -glucopyranosylpresenegenin 28- O -β- d -apiofuranosyl-(1 → 3)-β- d -xylopyranosyl-(1 → 4)-[β- d -apiofuranosyl-(1 → 3)]-α- l -rhamnopyranosyl-(1 → 2)-[(6- O -acetyl)-β- d -glucopyranosyl-(1 → 3)]-{4- O -[( E )-3,4,5-trimethoxycinnamoyl]}-β- d -fucopyranosyl ester, 3- O -β- d -glucopyranosylpresenegenin 28- O -β- d -apiofuranosyl-(1 → 3)-β- d -xylopyranosyl-(1 → 4)-[β- d -apiofuranosyl-(1 → 3)]-α- l -rhamnopyranosyl-(…
ChemInform Abstract: Preparation and Structural Characterization of (Me3SiNSN)2Se, a New Synthon for Sulfur-Selenium Nitrides.
2010
The reaction of (Me(3)SiN)(2)S with SeCl(2) (2:1 ratio) in CH(2)Cl(2) at -70 degrees C provides a route to the novel mixed selenium-sulfur-nitrogen compound (Me(3)SiNSN)(2)Se (1). Crystals of 1 are monoclinic and belong the space group P2(1)/c, with a = 7.236(1) A, b = 19.260(4) A, c = 11.436(2) A, beta = 92.05(3) degrees, V = 1592.7(5) A(3), Z = 4, and T = -155(2) degrees C. The NSNSeNSN chain in 1 consists of Se-N single bonds (1.844(3) A) and S=N double bonds (1.521(3)-1.548(3) A) with syn and anti geometry at the N=S=N units. The N-Se-N bond angle is 91.8(1) degrees. The EI mass spectrum shows a molecular ion with good agreement between the observed and calculated isotopic distributions…
Polymorphic and solvate structures of ethyl ester and carboxylic acid derivatives of WIN 61893 analogue and their stability in solution
2014
3-Ethyl ester- (1) and 3-carboxylic acid-isoxazole (2) derivatives of an antiviral drug analogue WIN 61893 were synthesized and characterized by X-ray crystallography and NMR spectroscopy. Crystallization experiments afforded two polymorphic structures for the ethyl ester derivative and two solvate structures for the carboxylic acid derivative based on their ability to form intermolecular hydrogen bonding interactions with the solvent molecules. The conformations of the derivatives depended greatly on the orientation of the planar isoxazole and phenyl-oxadiazole ring systems with respect to one another and were found to take up perpendicular, linear or tilted conformations. The carboxylic a…
Omphalotins E-I, Five Oxidatively Modified Nematicidal Cyclopeptides fromOmphalotus olearius
2009
Omphalotins E–I, oxidatively modified cyclic dodecapeptides, were isolated from mycelial extracts of the basidiomycete Omphalotus olearius, and their structures were determined by NMR spectroscopic and MS methods. Four of the five omphalotins contained an unprecedented N-hydroxylated tricyclic tryptophan derivative. All compounds exhibited strong and selective nematicidal activity against the plant pathogen Meloidogyne incognita with LD90 values between 2 and 5 μg mL–1. Cytotoxic activities were not detected up to 50 μg mL–1. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009)
Synthesis and Characterization of theO-Alkylation Products of Resorcinarene
2013
O-Substitution reactions of tetramethoxyresorcinarene with alkyl halides produced a variety of partially O-alkylated resorcinarene derivatives with terminal alkyne functionality. The degree of alkylation was affected by the reactivity of the alkylating halide used. NMR spectroscopy proved to be an ideal tool for analyzing the complex reaction mixtures and the isolated products based on the symmetry and degree of alkylation of the resorcinarene derivatives. Single-crystal X-ray diffraction studies furthermore showed diversity in the self-assembly of the various O-alkylation products that was greatly affected by the degree of alkylation, as well as the nature of the alkyne moiety.
Synthesis and characterisation of tetrazole compounds: 3 series of new ligands representing versatile building blocks for iron(II) spin-crossover com…
2005
Abstract New tetrazole compounds were synthesized and characterised by NMR and FTIR spectroscopy as well as by single crystal X-ray diffraction. We present in this paper mono- and ditetrazoles, which represent a versatile class of building blocks for the formation of mononuclear iron(II) complexes with monotetrazoles as terminal ligands as well as iron(II) coordination polymers with ditetrazoles as bridging ligands. Especially, the series of α,ω-bis[tetrazol-1-yl]-alkanes open the field of fascinating supramolecular structures with spin transition properties.
1H,13C and17O NMR spectroscopic study of four bicyclo [3.1.1]heptenes (derivatives of α-pinene) and four bicyclo[3.1.1]heptanes (derivatives of β-pin…
1992
Four derivatives of 2, 6, 6-trimethylbicyclo[3.1.1]hept-2-ene (α-pinene) and four derivatives of 2-methylene-6, 6-dimethylbicyclo[3.1.1]heptane (β-pinene) were synthesized and their 1H, 13C and 17O NMR spectra were measured, analysed and assigned. The 1H NMR spectral parameters were obtained by computer-aided analyses of the very complex multi-spin, second-order spectra. Some of the 13C NMR chemical shift assignments of these compounds reported in the literature should be changed, based on these accurate 1H NMR spectral analyses and carbon-proton chemical shift correlated spectra (COSY). The new assignments are supported by the 1J(C, H) values, which show a strong dependence on the bond ang…