共查询到20条相似文献,搜索用时 15 毫秒
1.
《Magnetic resonance in chemistry : MRC》2002,40(7):480-482
1H, 13C and 15N NMR chemical shifts of 10 substituted pyrazolo[1,5‐a]pyrimidines were assigned based on DQF 1H, 1H COSY, PFG 1H, 13C HMQC and PFG 1H,X (X = 13C and 15N) HMBC experiments and on literature data. Copyright © 2002 John Wiley & Sons, Ltd. 相似文献
2.
Tousek J Van Miert S Pieters L Van Baelen G Hostyn S Maes BU Lemière G Dommisse R Marek R 《Magnetic resonance in chemistry : MRC》2008,46(1):42-51
Indoloquinoline alkaloids represent an important class of antimalarial, antibacterial and antiviral compounds. They have been shown to bind to DNA via intercalation preferentially at GC-rich sequences containing nonalternating CC sites. The stability of complexes formed with biological macromolecules depends on noncovalent binding. In the present study, the ability of indoloquinolines to form intermolecular interactions with solvents was investigated by using NMR spectroscopy and density functional theory (DFT) (B3LYP/6-31G**) calculations. NMR data measured for indoloquinoline bases and the corresponding hydrochlorides are discussed in relation to the structure. DFT calculations of shielding constants in vacuo and in solution allowed the investigation of the influence of the environment on the NMR parameters. Calculations incorporating solvent effects indicated significant changes in the anisotropy of the electron distribution, reflected in the span of the chemical shielding tensor (Omega = sigma11 - sigma33). Solvent effects on the span of the 13C and 15N shielding tensor depended on the type of atom and the data indicated a significant influence of solute-solvent interactions. 相似文献
3.
1H NMR assignment, including the values of delta(H) and J(H,H) for the cyclopropane moiety, and 13C NMR and 15N NMR spectral data for ciprofloxacin are presented. 相似文献
4.
1H, 13C and 15N NMR measurements (1D and 2D including 1H--15N gs-HMBC) have been carried out on 3-amino-1, 2,4-benzotriazine and a series of N-oxides and complete assignments established. N-Oxidation at any position resulted in large upfield shifts of the corresponding N-1 and N-2 resonances and downfield shifts for N-4 with the exception of the 3-amino-1,2,4-benzotriazine 1-oxide in which a small upfield shift of N-4 was observed. Density functional GIAO calculations of the 15N and 13C chemical shifts [B3LYP/6-31G(d)//B3LYP/6-311+G(2d,p)] gave good agreement with experimental values confirming the assignments. The combination of 13C and 15N NMR provides an unambiguous method for assigning the 1H and 13C resonances of N-oxides of 1,2,4-benzotriazines. 相似文献
5.
Wolfgang Holzer Gernot A. Eller Barbara Datterl Daniela Habicht 《Magnetic resonance in chemistry : MRC》2009,47(7):617-624
NMR spectroscopic studies are undertaken with derivatives of 2‐pyrazinecarboxylic acid. Complete and unambiguous assignment of chemical shifts (1H, 13C, 15N) and coupling constants (1H,1H; 13C,1H; 15N,1H) is achieved by combined application of various 1D and 2D NMR spectroscopic techniques. Unequivocal mapping of 13C,1H spin coupling constants is accomplished by 2D (δ,J) long‐range INEPT spectra with selective excitation. Phenomena such as the tautomerism of 3‐hydroxy‐2‐pyrazinecarboxylic acid are discussed. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
6.
Schofield MH Sorel MA Manalansan RJ Richardson DP Markgraf JH 《Magnetic resonance in chemistry : MRC》2006,44(9):851-855
The synthesis and assignment of 15N and 13C NMR signals of the isoxazole ring in a series of para-substituted 3-phenyl derivatives are reported. DFT calculations of 15N and 13C chemical shifts are presented and compared to observed values. Substituent effects are interpreted in terms of the Hammett correlation and calculated bond orders. 相似文献
7.
Pascal Palmas Coralie Nyffenegger Eric Pasquinet Gérald Guillaumet 《Magnetic resonance in chemistry : MRC》2009,47(9):752-756
Mesomeric heteropentalene betaines are conjugated fused polyheterocyclic structures that represent interesting intermediates for organic synthesis. Five such structures, containing at least four nitrogen atoms and various substituents, have been characterized by 1H, 13C and 15N NMR. We report, apparently for the first time, nitrogen NMR data and coupling information on such systems. Inter‐ring long‐range correlations across five bonds with 15N (5JHN) and up to seven bonds with 13C (6JHC and 7JHC) were observed in HSQC experiments. The incorporation of an electron‐withdrawing substituent such as NO2 was observed to cause an increase in the magnitude of the remote couplings and deshielding of nearby protons, carbons and on all nitrogen atoms of the structure, including remote ones situated on other cycles. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
8.
The complete (1)H, (13)C and (15)N NMR signals assignment of adenosine derivatives differently substituted at C(6)-position was achieved using one- and two-dimensional experiments (gs-COSY, gs-NOESY, gs-HSQC and gs-HMBC). 相似文献
9.
Markgraf JH Hong L Richardson DP Schofield MH 《Magnetic resonance in chemistry : MRC》2007,45(11):985-988
The synthesis and assignment of (15)N and (13)C NMR signals of the 1,3,4-oxathiazol-2-one ring in a series of para-substituted 5-phenyl derivatives are reported. DFT calculations of (15)N and (13)C chemical shifts correspond closely to observed values. Substituent effects are interpreted in terms of the Hammett correlation and calculated bond orders. 相似文献
10.
Silvana Casati Ada Manzocchi Roberta Ottria Pierangela Ciuffreda 《Magnetic resonance in chemistry : MRC》2010,48(9):745-748
The complete 1H, 13C and 15N NMR signals assignments of some new isopentenyladenosine analogues were achieved using one‐ and two‐dimensional experiments (gs‐NOESY, gs‐HMQC and gs‐HMBC). Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
11.
Leszek Pazderski Jaromír Toušek Jerzy Sitkowski Kateřina Maliňáková Lech Kozerski Edward Szłyk 《Magnetic resonance in chemistry : MRC》2009,47(3):228-238
1H, 13C and 15N NMR studies of gold(III), palladium(II) and platinum(II) chloride complexes with picolines, [Au(PIC)Cl3], trans‐[Pd(PIC)2Cl2], trans/cis‐[Pt(PIC)2Cl2] and [Pt(PIC)4]Cl2, were performed. After complexation, the 1H and 13C signals were shifted to higher frequency, whereas the 15N ones to lower (by ca 80–110 ppm), with respect to the free ligands. The 15N shielding phenomenon was enhanced in the series [Au(PIC)Cl3] < trans‐[Pd(PIC)2Cl2] < cis‐[Pt(PIC)2Cl2] < trans‐[Pt(PIC)2Cl2]; it increased following the Pd(II) → Pt(II) replacement, but decreased upon the trans → cis‐transition. Experimental 1H, 13C and 15N NMR chemical shifts were compared to those quantum‐chemically calculated by B3LYP/LanL2DZ + 6‐31G**//B3LYP/LanL2DZ + 6‐31G*. Copyright © 2008 John Wiley & Sons, Ltd. 相似文献
12.
《Magnetic resonance in chemistry : MRC》2003,41(7):541-544
Treatment of 2‐acetyl‐2‐methylcyclopentanone with hydrazine hydrate yielded a new condensed hexahydro‐1,3,5‐triazine (3b), which is the first example of the ketimine‐type trimers. A complete 1H, 13C and 15N NMR assignment of the compound was achieved. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
13.
Alan R. Katritzky Bahaa El‐Dien M. El‐Gendy Bogdan Draghici Dmytro Fedoseyenko Aziz Fadli Eric Metais 《Magnetic resonance in chemistry : MRC》2010,48(5):397-402
1H, 13C, and 15N NMR chemical shifts for pyridazines 4–22 were measured using 1D and 2D NMR spectroscopic methods including 1H? 1H gDQCOSY, 1H? 13C gHMQC, 1H? 13C gHMBC, and 1H? 15N CIGAR–HMBC experiments. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
14.
Eliška Procházková Michal Šála Radim Nencka Martin Dračínský 《Magnetic resonance in chemistry : MRC》2012,50(3):181-186
We measured the 1H, 13 C and 15 N chemical shifts for a series of purine derivatives bearing a norbornane substituent in position 9 and various substituents in position 6. The experimental data were complemented with density functional theory (DFT) calculations. The comparison of the calculated and experimental chemical shifts provided us with information about the tautomer and conformational equilibria of the studied compounds. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
15.
Roberta Ottria Silvana Casati Pierangela Ciuffreda 《Magnetic resonance in chemistry : MRC》2012,50(12):823-828
The complete 1H, 13C and 15N NMR signal assignments of some N‐ and O‐acylethanolamines, important family of naturally occurring bioactive lipid mediators, were achieved using one‐dimensional and two‐dimensional experiments (gs‐HMQC and gs‐HMBC). Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
16.
Claramunt RM Santa María MD Sanz D Alkorta I Elguero J 《Magnetic resonance in chemistry : MRC》2006,44(5):566-570
Three N-substituted pyrazoles and three N-substituted indazoles [1-(4-nitrophenyl)-3,5-dimethylpyrazole (1), 1-(2,4-dinitrophenyl)-3,5-dimethylpyrazole (2), 1-tosyl-pyrazole (3), 1-p-chlorobenzoylindazole (4), 1-tosylinda-zole (5) and 2-(2-hydroxy-2-phenylethyl)-indazole (6)] have been studied by NMR spectroscopy in solution (1H, 13C, 15N) and in the solid state (13C, 15N). The chemical shifts have been compared with GIAO/DFT calculated absolute shieldings. Some discrepancies have been analyzed. 相似文献
17.
The 1H, 13C, 15N and 19F NMR spectra of nine DL-phenylalcoholamides bearing fluorine and chlorine as substituents of the phenyl ring are reported. All of them are active as anticonvulsants in pentylenetetrazole-induced seizures. 相似文献
18.
The 1H and 13C NMR resonances of 15 N,N'-diacylproflavines were assigned completely and unequivocally using a concerted application of one- and two-dimensional experiments (DEPT, gs-COSY, gs-HMQC and gs-HMBC). 相似文献
19.
20.
The effects of including (a) implicit solvent in geometry optimizations, (b) conformationally flexible molecules in test sets, and (c) empirical dispersion D3(BJ) on scaling factors for predicting 1H and 13C NMR chemical shifts were explored. Scaling factors with optimizations performed in the gas phase and with a Polarizable Continuum Model (PCM) solvent model were obtained for 12 organic solvents, including 2,2,2-trifluroethanol and chlorobenzene, for which scaling factors have been developed for the first time. Scaling factors for aromatic solvents were split into primary and secondary scaling factors to account for CH–π effects. Including empirical dispersion D3(BJ) did not lead to significant improvement. 相似文献