共查询到20条相似文献,搜索用时 15 毫秒
1.
Compounds 1-7 form a novel group of dithiocarbamates, first synthesized from the reaction of a series of primary amines with carbon disulfide and 3-bromo ethyl pyruvate in the presence of anhydrous potassium phosphate. Structure elucidation of this group of compounds was accomplished using extensive 1D and 2D NMR spectroscopic studies, including (1)H, (13)C, COSY, NOESY, HSQC, and gHMBC experiments. The distinction between the linear structures I, II and the cyclic structure III was made mainly on the basis of the analysis of the cross peak between H-2 and H-4a in the COSY spectra, in combination with the long-range correlation between H-2 and C-4, 6 in the gHMBC spectra. 相似文献
2.
Data from two-dimensional (2D) NMR experiments were used to identify the reaction products resulting from the opening of pyroglutamates with isocyanates or thioisocyanates. The reaction has the potential to produce compounds that would have very similar one-dimensional proton ((1)H) or carbon-13 ((13)C) NMR spectra. Careful analysis of (1)H--(1)H COSY, (1)H--(1)H NOESY, and HMBC data, including chemical shifts and coupling constants, were used to distinguish correctly between carbamoyl-2-pyrrolidinone, hydantoin, and perhydro-1,3-diazepine-2,4-dione type structures that could result from this reaction. This work describes their preparation and subsequent identification using 2D NMR spectroscopy, and includes complete (13)C assignments of the reaction products. The 2D NMR techniques and analysis described here can be applied successfully to other synthetic reactions with the potential to produce isomeric products. 相似文献
3.
Hossein Reza Darabi Marjan Azimzadeh Arani Mohsen Tafazzoli Mina Ghiasi 《Monatshefte für Chemie / Chemical Monthly》2008,139(10):1185-1189
The existence of a short C–H ⋯ π (alkyl–alkyne) interaction in the structure of a strained and relatively rigid tolanophane
is expected to hinder the rotation about the C–C sp3 single bond. Variable-temperature NMR experiments (performed in three solvents, CDCl3, THF-d8, and acetone-d6) and ab initio density functional calculations were carried out to investigate its dynamic nature. An energy barrier of 48.6 kJ/mol is determined
at coalescence (210 K) with acetone-d6 which is in good agreement with calculation result (54 kJ/mol).
Correspondence: Hossein Reza Darabi, Chemistry and Chemical Engineering Research Center of Iran, Pajoohesh Blvd., km 17, Karaj
Hwy, 14968-13151 Tehran, Iran. 相似文献
4.
Kun Zou Jun‐zhi Wang Zhi‐yong Guo Ming Du Jun Wu Yuan Zhou Fei‐jun Dan Chuang Liu 《Magnetic resonance in chemistry : MRC》2009,47(1):87-91
Four new furostanol saponins (1–4), two pairs of diastereoisomers, were isolated from methanolic extracts of Tupistra chinensis rhizomes and their structures were assigned from 1H and 13C NMR spectra, DEPT, and by 2D COSY, NOESY, HMQC, and HMBC experiments. Copyright © 2008 John Wiley & Sons, Ltd. 相似文献
5.
Muhammad Imran Muhammad Ibrahim Naheed Riaz Prof. Dr. Abdul Malik 《Magnetic resonance in chemistry : MRC》2009,47(6):532-536
Aervins A‐D (1‐4), four new coumaronochromone analogues have been isolated from the CHCl3‐soluble fraction of the MeOH extract of the whole plant of Aerva persica. Their structures were assigned based on 1H NMR, 13C NMR spectra, DEPT, and by 2DNMR experiments. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
6.
Ultrafast 2D NMR allows the acquisition of a 2D spectrum in a single scan. However, even when the acquisition of ultrafast spectra is carried out under optimized conditions, the appearance and the sensitivity of 2D spectra are often not satisfactory compared with what one could expect from this promising methodology. This is due to limitations in terms of sensitivity, spectral width and resolution, and also to non-ideal lineshapes characterized by asymmetric sinc wiggles. Here, we identify the origin of these distortions by means of numerical simulations compared with experimental data. We then propose a processing approach to improve lineshapes while increasing the sensitivity of ultrafast experiments. The method consists in multiplying the Fourier transform of ultrafast echoes by an optimized apodization function. The principles of the method are described, and a variety of window functions are tested to determine optimum processing conditions. The approach is finally applied to ultrafast 2D spectra, leading to symmetric lineshapes with a sensitivity increased by a factor of 2. 相似文献
7.
Atricins A (1) and B (2), two new oleanane-type triterpenes have been isolated from the chloroform-soluble fractions of Perovskia atriplicifolia and their structures assigned from (1)H and (13)C-NMR spectra, Distortion Enhancement by Polarization Trasfer (DEPT) and by 2D-COSY, HMQC, Nuclear Overhauser Enhancement Spectroscopy (NOESY) and Hetronuclear mutiple-bond correlation (HMBC) experiments. 相似文献
8.
Cruz-López O Gallo MA Espinosa A Campos JM 《Magnetic resonance in chemistry : MRC》2007,45(2):185-188
The 1H and 13C NMR resonances of thirty 2-functionalized 5-(methylsulfonyl)-1-phenyl-1H-indoles were assigned completely and unequivocally using the concerted application of one- and two-dimensional experiments (DEPT, gs-HMQC and gs-HMBC). Finally, the influence of the 2-substituent of 5-(methylsufonyl)-1-phenyl-1H-indoles on the carbon atoms of the indole moiety was estimated. 相似文献
9.
Bakhat Ali Muhammad Imran Riaz Hussain Zaheer Ahmed Abdul Malik 《Magnetic resonance in chemistry : MRC》2010,48(2):159-163
Two new flavonoids, abutilin A and B, were isolated from the chloroform soluble fraction of Abutilon pakistanicum and their structures assigned from 1H and 13C NMR spectra, DEPT and by 2D COSY, HMQC and HMBC experiments. Ferulic acid (3), (E)‐cinnamic acid (4), 5‐hydroxy‐4′,6,7,8‐tetramethoxyflavone (5), kaempferol (6), luteolin (7) and luteolin 7‐O‐β‐D ‐glucopyranoside (8) have also been reported from this species. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
10.
Structural determination of kochiosides A-C, new steroidal glucosides from Kochia prostrata, by 1D and 2D NMR spectroscopy 总被引:1,自引:0,他引:1
Kochiosides A-C, three new steroidal glucosides, have been isolated from the ethyl acetate fraction of Kochia prostrata and their structures assigned from its (1)H and (13)C NMR spectra, DEPT and by 2D COSY, NOESY, HMQC and HMBC experiments. 相似文献
11.
Silymins A (1) and B (2), the new pentacyclic triterpenes, have been isolated from ethyl acetate fraction of Silybum marianum and their structures assigned from 1H and 13C NMR spectra, DEPT and by 2D COSY, NOE and HMBC experiments. 相似文献
12.
Burgueño-Tapia E Hernández LR Reséndiz-Villalobos AY Joseph-Nathan P 《Magnetic resonance in chemistry : MRC》2004,42(10):887-892
Extensive application of 1D and 2D NMR methodology, combined with molecular modeling, allowed the complete 1H and 13C NMR assignments of eremophilanolides from Senecio toluccanus. Comparison of the experimental 1H, 1H coupling constant values with those generated employing a generalized Karplus-type relationship, using dihedral angles extracted from MMX and DFT calculations, revealed that the epoxidized eremophilanolides 1 and 2 show conformational rigidity at room temperature, whereas molecules 3-6, containing an isolated double bond, are conformationally mobile. 相似文献
13.
Alexandra Gaspar Fernando Cagide Elias Quezada Joana Reis Eugenio Uriarte Fernanda Borges 《Magnetic resonance in chemistry : MRC》2013,51(4):251-254
Chromones are heterocyclic compounds of natural or synthetic origin that possess relevant pharmacological activities. Versatile functionalization of the chromone nucleus allows attaining of a chemical diversity suitable to perform structure–activity relationships in drug discovery and development programs. Accordingly, the synthesis and identification of novel chromone carboxamide derivatives with electron‐donating and electron‐withdrawing substituents in different positions of the exocyclic ring are reported in this work. Their complete structural characterization was performed using one‐dimensional and two‐dimensional resonance techniques. The data acquired are useful for a prompt analysis of related compounds that encompass our integrated medicinal chemistry sketch. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
14.
Arnaud Bondon Marie Autret Gérard Simonneaux 《Magnetic resonance in chemistry : MRC》1994,32(2):78-82
The efficiency of two-dimensional homonuclear 1H 1H NOE spectroscopy in characterizing and fully assigning the 1H NMR spectra of several isomers of meso- or ring-substituted deuteroporphyrins is demonstrated. The carbon resonances of the skeleton and the substituents were fully assigned using two-dimensional reverse heteronuclear shift correlation spectroscopy. 相似文献
15.
Trifunović S Milosavljević S Vajs V Macura S Todorović N 《Magnetic resonance in chemistry : MRC》2008,46(5):427-431
From detailed study of 1D and 2D NMR spectra of ten natural 1,2-epoxyguaianolides (bis-1,2:3,4-epoxyguaianolides and guaianolide-1,2-epoxychlorohydrins), we identified general spectral traits helpful for stereochemical assignment of such sesquiterpene lactones. We found that the chemical shifts of certain (1)H and (13)C nuclei are consistently dependent on the configuration of 1,2-epoxy-ring which could be used as a simple rule for establishing this configuration. Then, from 1D and 2D (COSY, NOESY, HMQC, HMBC) NMR data, applying the observed rule, the structure and stereochemistry of two new, diastereomeric guaianolide-1,2-epoxychlorohydrins, isolated from Achillea serbica, are determined. The NMR data, namely, nuclear overhauser enhancement (NOE) correlations, pointed out two conformations of guaianolide's cycloheptane ring. The semiempirical calculations (AM1 and PM3 methods), performed in order to gain additional information regarding conformations, resulted in three geometries of investigated lactones. Even so, the conformations derived from the NMR data agreed well with those calculated by semiempirical methods. 相似文献
16.
Kazmi MH Ahmed E Hameed S Malik A Ashraf M 《Magnetic resonance in chemistry : MRC》2007,45(5):416-419
Two new pentacyclic triterpenes, sorbinols A (1) and B (2) have been isolated from the ethyl acetate fraction of Sorbus cashmariana and their structures assigned from (1)H and (13)C NMR spectra, DEPT and by 2D COSY, NOE, HMQC and HMBC experiments. Both 1 and 2 showed moderate inhibitory potential against the enzyme lipoxygenase. 相似文献
17.
18.
《Magnetic resonance in chemistry : MRC》2003,41(2):115-122
3α‐Acetyl‐β‐boswellic acid ( 1 ), 3α‐acetyl‐α‐boswellic acid ( 2 ), 3α‐acetyl‐9,11‐dehydro‐β‐boswellic acid ( 3 ), 3α‐acetyl‐9,11‐dehydro‐α‐boswellic acid ( 4 ) and 3α‐acetyl‐11‐keto‐β‐boswellic acid ( 5 ) were isolated from the gum resin of Boswellia serrata. 1D and 2D NMR (COSY45, HMQC, HMBC, ROESY) spectra at 500 MHz were used for shift assignments and structure verification. All boswellic acids investigated share the cis conformation at ring D/E and the 3α orientation of the acetyl ester group. Owing to high‐order spectra, NMR could not determine the exact conformation of H‐20/H‐30 of the β‐boswellic acids. 3α‐Acetyl‐β‐boswellic acid methyl ester ( 1 ′) was synthesized for experiments with a shift reagent, Eu(fod)3, that enhanced the resolution considerably. The oxygen atoms of the 3α‐acetyl group form the apparent complex binding site for the shift reagent. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
19.
Ahmad Z Mehmood S Fatima I Malik A Ifzal R Afza N Iqbal L Latif M Nizami TA 《Magnetic resonance in chemistry : MRC》2008,46(1):94-98
Salsolins A (1) and B (2), the new triterpenes, have been isolated from the chloroform soluble fraction of Salsola baryosma along with 2alpha,3beta,23,24-tetrahydroxyurs-12-en-28-oic acid (3) reported for the first time from this species. Their structures have been assigned from 1H and 13C NMR spectra, DEPT and by 2D COSY, NOESY, HMQC and HMBC experiments. The compounds 1-3 showed significant antioxidant activity. 相似文献
20.
We present the results from a Comparative Molecular Field Analysis (CoMFA) and docking study of a diverse set of 36 estrogen receptor ligands whose relative binding affinities (RBA) with respect to 17-Estradiol were available in both isoforms of the nuclear estrogen receptors (ER, ER). Initial CoMFA models exhibited a correlation between the experimental relative binding affinities and the molecular steric and electrostatic fields; ER: r2=0.79, q2=0.44 ER: r2=0.93, q2=0.63. Addition of the solvation energy of the isolated ligand improved the predictive nature of the ER model initially; r2=0.96, q2=0.70 but upon rescrambling of the data-set and reselecting the training set at random, inclusion of the ligand solvation energy was found to have little effect on the predictive nature of the CoMFA models. The ligands were then docked inside the ligand binding domain (LBD) of both ER and ER utilizing the docking program Gold, after-which the program CScore was used to rank the resulting poses. Inclusion of both the Gold and CScore scoring parameters failed to improve the predictive ability of the original CoMFA models. The subtype selectivity expressed as RBA(ER/ER) of the test sets was predicted using the most predictive CoMFA models, as illustrated by the cross-validated r2. In each case the most selective ligands were ranked correctly illustrating the utility of this method as a prescreening tool in the development of novel estrogen receptor subtype selective ligands. 相似文献