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1.
《Magnetic resonance in chemistry : MRC》2002,40(7):467-470
In the course of saponification experiments with bis(2‐cyanoethyl) 2,6‐dimethyl‐4‐(2‐nitrophenyl)‐1,4‐dihydro‐3,5‐pyridinedicarboxylate ( 1 ), an analogue of the calcium channel blocker nifedipine, three unexpected degradation products were isolated. The compounds were identified as 3‐(2‐acetamido‐1‐carboxy‐1‐propenyl)‐1‐hydroxy‐2‐indolecarboxylic acid ( 3 ), 9‐hydroxy‐1,3‐dimethyl‐β‐carboline‐4‐carboxylic acid ( 4 ) and 6‐hydroxy‐2,4‐dimethyl‐5‐oxo‐5,6‐dihydrobenzo[c][2,7]naphthyridine‐1‐carboxylic acid ( 6 ). The structures of these compounds were deduced from one‐ and two‐dimensional 1H, 13C and natural abundance 15N NMR experiments (1H,1H‐COSY, gs‐HSQC, gs‐HMBC, 15N gs‐HMBC), and corroborated by comparison of their NMR data with the respective data for structurally similar compounds. Copyright © 2002 John Wiley & Sons, Ltd. 相似文献
2.
《Magnetic resonance in chemistry : MRC》2003,41(7):549-553
The1H and 13C NMR resonances for acridine derivatives 9‐substituted with chloro, allylamino and propargylamino groups were completely assigned using a concerted application of gs‐COSY, gs‐HMQC and gs‐HMBC experiments. 9‐(N‐Allyl)‐ and 9‐(N‐propargyl)acridinamine derivatives present amino–imino tautomerism including a large broadening of 1H and 13C NMR signals at room temperature. To obtain suitable resolution, therefore, these latter compounds were studied at 370 K in DMSO‐d6 solutions and showed a complete shift towards the imino tautomers. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
3.
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
4.
M. Dora Carrión Mariem Chayah Duane Choquesillo‐Lazarte Miguel A. Gallo Antonio Espinosa Antonio Entrena M. Encarnación Camacho 《Magnetic resonance in chemistry : MRC》2012,50(1):58-61
The 13 C NMR resonances of 19 1‐acyl‐3‐(2‐nitro‐5‐substitutedphenyl)‐4,5‐dihydro‐1H‐pyrazoles, and 19 1‐acyl‐3‐(2‐amino‐5‐substituted)‐4,5‐dihydro‐1H‐pyrazoles, were completely assigned using the concerted application of one‐ and two‐dimensional NMR experiments (DEPT, gs‐HSQC and gs‐HMBC). Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
5.
Luisa C. López‐Cara M. José Pineda de las Infantas M. Dora Carrión M. Encarnación Camacho Miguel A. Gallo Antonio Espinosa Antonio Entrena 《Magnetic resonance in chemistry : MRC》2009,47(12):1101-1109
The 1H and 13C NMR resonances of 22 5‐(5‐substituted‐2‐nitrophenyl)‐1H‐pyrrole‐2‐carboxamides, 22 5‐(5‐substituted‐2‐aminophenyl)‐1H‐pyrrole‐2‐carboxamides, and 9 5‐phenyl‐1H‐pyrrole‐2‐carboxamides were assigned completely using the concerted application of one‐ and two‐dimensional experiments (DEPT, gs‐HMQC and gs‐HMBC). NOE studies and conformational analysis confirm the preferred conformations of such compounds. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
6.
《Magnetic resonance in chemistry : MRC》2002,40(8):545-548
The 1H and 13C NMR resonances for 16 acridin‐9(10H)‐ones substituted with amino or (1,3‐benzothiazol‐2‐yl)amino groups were completely and unequivocally assigned by the concerted application of gs‐COSY, gs‐HMQC and gs‐HMBC experiments. Evidence for hydrogen bond and amino–imino tautomerism is presented for 1‐ and 4‐substituted acridin‐9(10H)‐ones. Copyright © 2002 John Wiley & Sons, Ltd. 相似文献
7.
Aline Lima de Oliveira Carlos Henrique Alves de Oliveira Laura Maia Mairink Francine Pazini Ricardo Menegatti Luciano Morais Lião 《Magnetic resonance in chemistry : MRC》2011,49(8):537-542
Complete assignment of 1H and 13C NMR chemical shifts and J(1H/1H and 1H/19F) coupling constants for 22 1‐phenyl‐1H‐pyrazoles' derivates were performed using the concerted application of 1H 1D and 1H, 13C 2D gs‐HSQC and gs‐HMBC experiments. All 1‐phenyl‐1H‐pyrazoles' derivatives were synthesized as described by Finar and co‐workers. The formylated 1‐phenyl‐1H‐pyrazoles' derivatives were performed under Duff's conditions. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
8.
A. S. Brar Rajeev Kumar 《Journal of polymer science. Part A, Polymer chemistry》2002,40(14):2225-2236
N‐vinyl‐2‐pyrrolidone/methyl acrylate (V/M) copolymers were prepared by free‐radical bulk polymerization using benzoyl peroxide as an initiator. The copolymer composition of these copolymers was calculated from 1H NMR spectra. The radical reactivity ratios for N‐vinyl‐2‐pyrrolidone (V) and methyl acrylate (M) were rV = 0.09, rM = 0.44. These reactivity ratios for the copolymerization of V and M were determined using the Kelen–Tudos and nonlinear least‐squares error‐in‐variable methods. The 13C{1H} and 1H NMR spectra of these copolymers overlapped and were complex. The complete spectral assignment of the 13C and 1H NMR spectra were done with distortionless enhancement by polarization transfer and two dimensional 13C‐1H heteronuclear single quantum correlation spectroscopic experiments. The two‐dimensional 1H‐1H homonuclear total correlation spectroscopic NMR spectrum showed the various bond interactions, thus inferring the possible structure of the copolymers. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 2225–2236, 2002 相似文献
9.
A. S. Brar Rajeev Kumar 《Journal of polymer science. Part A, Polymer chemistry》2002,40(15):2717-2717
N‐vinyl‐2‐pyrrolidone/methyl acrylate (V/M) copolymers were prepared by free‐radical bulk polymerization using benzoyl peroxide as an initiator. The copolymer composition of these copolymers was calculated from 1H NMR spectra. The radical reactivity ratios for N‐vinyl‐2‐pyrrolidone (V) and methyl acrylate (M) were rV = 0.09, rM = 0.44. These reactivity ratios for the copolymerization of V and M were determined using the Kelen–Tudos and nonlinear least‐squares error‐in‐variable methods. The 13C{1H} and 1H NMR spectra of these copolymers overlapped and were complex. The complete spectral assignment of the 13C and 1H NMR spectra were done with distortionless enhancement by polarization transfer and two dimensional 13C‐1H heteronuclear single quantum correlation spectroscopic experiments. The two‐dimensional 1H‐1H homonuclear total correlation spectroscopic NMR spectrum showed the various bond interactions, thus inferring the possible structure of the copolymers. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 2225–2236, 2002 相似文献
10.
Rafael Germano Santana Derisvaldo Rosa Paiva Roberto da Silva Gomes Adriana Karla C. A. Reis 《Magnetic resonance in chemistry : MRC》2013,51(5):316-319
The complete assignment of the 1H and 13C NMR spectra of various 2‐acetamido‐3‐mercapto‐3‐methyl‐N‐aryl‐butanamides and 2‐acetamide‐3‐methyl‐3‐nitrososulfanyl‐N‐aryl‐butanamides with p‐methoxy, o‐chloro and m‐chloro substituents is reported. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
11.
Jan Vícha Michal Maloň Petra Veselá Otakar Humpa Miroslav Strnad Radek Marek 《Magnetic resonance in chemistry : MRC》2010,48(4):318-322
The 1H and 13C NMR resonances of 16 purine glucosides were assigned by a combination of one‐ and two‐dimensional NMR experiments, including gs‐COSY, gs‐HSQC, and gs‐HMBC, in order to characterize the effect of substituent and the position of glucose unit on the NMR chemical shifts. In addition, 15N NMR chemical shifts for selected derivatives were investigated by using 1H? 15N chemical shift correlation techniques. To map the influence of sugar moiety on the directly bonded nitrogen atom, selected N9‐glucosides and their ribose analogs were compared. Characteristic long‐range 1H? 15N coupling constants, measured by using 1H? 15N gradient‐selected single‐quantum multiple bond correlation (GSQMBC), are also reported and discussed. All compounds investigated here belong to cytokinins, an important group of plant hormones. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
12.
Valerie Huemer Gernot A. Eller Wolfgang Holzer 《Magnetic resonance in chemistry : MRC》2010,48(6):476-482
Various [5,6]pyrano[2,3‐c]pyrazol‐4(1H)‐thiones were synthesized in high yields by treatment of the corresponding [5,6]pyrano[2,3‐c]pyrazol‐4(1H)‐ones with Lawesson's reagent. Detailed NMR spectroscopic studies were undertaken of the title compounds. Complete and unambiguous assignment of chemical shifts (1H, 13C, 15N) and coupling constants (1H,1H; 13C,1H) was achieved by the combined application of various one‐ and two‐dimensional (1D and 2D) NMR spectroscopic techniques. Unequivocal mapping of most 13C,1H spin coupling constants is accomplished by 2D (δ, J) long‐range INEPT spectra with selective excitation. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
13.
《Magnetic resonance in chemistry : MRC》2003,41(4):301-303
4‐Methyl‐6,8‐dihydroxy‐7H‐benz[de]anthracen‐7‐one was isolated from the sap of Aloe by column chromatography. Its 1H and 13C NMR spectra were completely assigned by utilizing two‐dimensional 1H‐detected heteronuclear one‐bond (HMQC) and multiple‐bond (HMBC) chemical shift correlation experiments together with 1H–1H COSY and DEPT techniques. These techniques were also valuable in assigning the protons and carbons of those benzanthrone compounds which were previously incompletely reported because of the overlap of proton signals. The molecular structure was elucidated by 2D NMR analysis. The spectral properties (MS, IR and UV) are also presented. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
14.
The complete 1H and 13C NMR signal assignments of 23 new N,N′‐diacyl proflavine derivatives were achieved using one‐ and two‐dimensional experiments (DEPT, HMQC and HMBC). Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
15.
Faten Al Chab Bernard Fenet Marc Le Borgne Joachim Jose Noël Pinaud Jean Guillon Laurent Ettouati 《Magnetic resonance in chemistry : MRC》2013,51(12):837-841
The complete 1H and 13C assignments of eight bioactive indeno[1,2‐b]indole‐10‐one derivatives were accomplished by the combined use of one‐dimensional and two‐dimensional NMR experiments. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
16.
《Magnetic resonance in chemistry : MRC》2003,41(9):721-725
The 1H, 13C and 15N NMR spectra in DMSO‐d6 were measured for eight nitraminopyridine N‐oxides, ten 4‐nitropyridine N‐oxides, four 2‐nitraminopyridines and five 4‐nitropyridines. Their chemical shift assignments are based on PFG 1H,X (X = 13C and 15N) HMQC and HMBC experiments. The relative energies for the tautomers of two nitraminopyridine N‐oxides were determined by ab initio HF/6–311G** calculations. A single‐crystal x‐ray structural analysis was made for 4‐methyl‐2‐nitraminopyridine: C6H7O2N3, M = 153.15, triclinic, space group P‐1 (No. 2), a = 7.0275(4), b = 6.8034(3), c = 8.6086(5) Å, α = 103.620(2), β = 90.309(2), γ = 122.215(3)°, V = 334.11(3) Å3, Z = 2. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
17.
Elena Bermejo Alfonso Castieiras Ricardo Domínguez Rosa Carballo Ccilia Maichle‐Mssmer Joachim Strhle Douglas X. West 《无机化学与普通化学杂志》1999,625(6):961-968
Reaction of group 12 metal dihalides in ethanolic media with 2‐acetylpyridine 4N‐phenylthiosemicarbazone ( H4PL ) and 2‐acetylpyridine‐N‐oxide 4N‐phenylthiosemicarbazone ( H4PLO ) afforded the compounds [M(H4PL)X2] (X = Cl, Br, M = Zn, Cd, Hg; X = I, M = Zn, Cd) ( 1–8 ), [Hg(4PL)I]2 ( 9 ) and [M(H4PLO)X2] (X = Cl, Br, I, M = Zn, Cd, Hg) ( 10–18 ). H4PL , H4PLO and their complexes were characterized by elemental analysis and by IR and 1H and 13C NMR spectroscopy (and the cadmium complexes by 113Cd NMR spectroscopy), and H4PL , H4PLO , ( 5 · DMSO) and ( 9 ) were additionally studied by X‐ray diffraction. H4PL is N,N,S‐tridentate in all its complexes, including 9 , in which it is deprotonated, and H4PLO is in all cases O,N,S‐tridentate. In all the complexes, the metal atoms are pentacoordinate and the coordination polyhedra are redistorted tetragonal pyramids. In assays of antifungal activity against Aspergillus niger and Paecilomyces variotii, the only compound to show any activity was [Hg(H4PLO)I2] ( 18 ). 相似文献
18.
《Magnetic resonance in chemistry : MRC》2003,41(12):1034-1037
The assignment of 1H and 13C NMR of the sesquiterpene (+)‐10β,14‐dihydroxy‐allo‐aromadendrane by means of two‐dimensional NMR is reported. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
19.
Ulrich Girreser Ullvi Bluhm Bernd Clement Dieter Heber 《Magnetic resonance in chemistry : MRC》2013,51(11):714-721
The NMR spectroscopic data of a series of thirty‐four 3‐acylpyrido[1,2‐a]pyrimidinium salts are analyzed, which were prepared as either perchlorates or chlorides. Methyl group substituted 3‐aroyltetrahydropyrido[1,2‐a]pyrimidines with the methyl substituent in positions 6, 8 and 9 as well as both in positions 6 and 8 were investigated bearing various aroyl substituents. Unequivocal assignment of all resonances was achieved via two‐dimensional 1H,1H‐COSY measurements, 1H,13C and 1H,15N HSQC as well as HMBC experiments, and important diagnostic CH and NH couplings in the heteroaromatic ring system are evaluated. The influence of the methyl substituents was analyzed on the proton, carbon and nitrogen shifts. A significant effect of the counter ion on some chemical shifts of the nuclei under discussion of the pyridopyrimidines is found, allowing the indirect detection of the anion, which is confirmed by direct measurement of the 35Cl nucleus of the perchlorates. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
20.
Nelson L. C. Domingues Paulo R. Olivato Adriana K. C. A. Reis Mirta G. Mondino Filipe S. Lima Roberto Rittner 《Magnetic resonance in chemistry : MRC》2009,47(3):270-272
The complete assignment of the 1H and 13C NMR spectra of the diastereomeric pairs of some α‐arylsulfinyl‐substituted N‐methoxy‐N‐methylpropionamides with the substituents methoxy, methyl, chloro, nitro is reported. Copyright © 2008 John Wiley & Sons, Ltd. 相似文献