119Sn, 15N, 13C, and 1H NMR Study of the Intramolecular Sn-N Donor-Acceptor Interaction in [2-(Dimethylaminomethyl)phenyl]stannanes

1998 ◽  
Vol 63 (7) ◽  
pp. 977-989 ◽  
Author(s):  
Aleš Růžička ◽  
Vladimír Pejchal ◽  
Jaroslav Holeček ◽  
Antonín Lyčka ◽  
Klaus Jacob
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Intramolecular Interaction ◽  
Coupling Constants ◽  
Acceptor Interaction ◽  
H Nmr ◽  
Nmr Parameters ◽  
Nmr Study ◽  
Donor Acceptor ◽  
Characteristic Values

119Sn, 15N, 13C, and 1H NMR spectra were studied for [2-(dimethylaminomethyl)phenyl]stannanes, R1R2R3R4Sn or R1R2R24Sn, where R1, R2, and R3 are 1-butyl, Cl or Br, the same or different, and R4 is 2-(dimethylaminomethyl)phenyl. The occurrence of intramolecular interaction between the nitrogen and tin atoms was demonstrated based on changes in the characteristic values of the NMR parameters of these nuclides (δ(15N), δ(119Sn), J(119Sn,15N), and their interrelations, as well as on the relatively high values of the coupling constants 3J(119Sn,13C(CH2)).

Das 7,8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ5-phosphaspiro[4.4]nonanyl-Kation: Röntgenstrukturanalyse und temperaturabhängige 1H-NMR-Spektren: The 7, 8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ).5-phosphaspiro[4.4]nonanyl Cation: X-Ray Crystal Structure Determination and Variable 1H NMR Spectra

1992 ◽  
Vol 47 (6) ◽  
pp. 755-759 ◽  
Author(s):  
Thomas Kaukorat ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crystal Structure ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Crystal Structure Analysis ◽  
Acceptor Interaction ◽  
Nmr Spectrum ◽  
X Ray ◽  
H Nmr ◽  
Trigonal Bipyramidal ◽  
Donor Acceptor

The 1H NMR spectrum of the spirophosphorane 3 at room temperature indicates dynamic behaviour of the cation. The low-temperature 1H NMR spectra of 3 exhibit two sets of doublets for the protons of the diastereotopic N(CH3)2 groups. The free enthalpy of activation for the dynamic process was determined (58.6 KJ/mole). In the reaction of 3 with sodium tetraphenylborate the crystalline compound, 4, involving the non-coordinating anion, [B(C6H5)4]-, was obtained. The X-ray crystal structure analysis of 4 reveals the presence of a five-membered ring, formally as a result of intramolecular donor-acceptor interaction between the nitrogen atom of the N(CH3)2 group and phosphorus. The geometry at phosphorus deviates somewhat from ideal trigonal bipyramidal.

A 15N, 13C, and 1H NMR study of reaction products from arylguanidines and chloroformate esters

1991 ◽  
Vol 56 (7) ◽  
pp. 1505-1511 ◽  
Author(s):  
Antonín Lyčka ◽  
Karel Palát
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Reaction Products ◽  
H Nmr ◽  
Nmr Study

The 15N, 13C, and 1H NMR spectra of the reaction products from arylguanidines with two mols of chloroformate esters have been measured. With application of the corresponding 15N isotopomer it has been proved that the reaction products have the structures IIIa-IIIc.

Wideline 1H NMR Study on Hydrated Layered Sulfides K0.5(H2O)y[NbS2] and Na0.5(H2O)y[NbS2]

1977 ◽  
Vol 32 (9) ◽  
pp. 1033-1037 ◽  
Author(s):  
Anton Lerf ◽  
Paul Burkert ◽  
Jürgen O. Besenhard ◽  
Robert Schöllhorn
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Interlayer Space ◽  
Water Molecules ◽  
Structural Scheme ◽  
H Nmr ◽  
Nmr Study

H NMR spectra of different hydration stages show that the water molecules in hydrated layered niobium sulfides A0.5(H2O)y[NbS2] are rather mobile at room temperature. A structural scheme of water arrangement in the interlayer space is proposed with the C2-axis of the H2O molecules parallel to the basal planes of the NbS2 layer units.

15N, 13C, and 1H NMR spectra of acylated ureas and thioureas

1987 ◽  
Vol 52 (10) ◽  
pp. 2474-2481 ◽  
Author(s):  
Josef Jirman ◽  
Antonín Lyčka
Keyword(s):  
1H Nmr ◽  
Electron Acceptor ◽  
Sulfur Atom ◽  
Nmr Spectra ◽  
Chemical Shifts ◽  
1H Nmr Spectra ◽  
Coupling Constants ◽  
Nmr Chemical Shifts ◽  
H Nmr ◽  
Better Than

A series of 1-acylated and 1,3-diacylated (acyl = acetyl or benzoyl) ureas and thioureas have been prepared and their proton-coupled and proton-decoupled 15N, 13C, and 1H NMR spectra have been measured. All the signals have been assigned. The 15N NMR chemical shifts in 1-acylated ureas and thioureas are shifted downfield as compared with δ(15N) of urea and thiourea, resp. This shift is greater for N-1 than for N-3 nitrogen atoms in both the series. When comparing acylureas and acylthioureas it is obvious from the Δδ(15N) differences that the CS group is better than CO group in transferring the electron-acceptor effect of acyl group. The proton-coupled 15N NMR spectra of the acylureas dissolved in hexadeuteriodimethyl sulphoxide exhibit a doublet of NH group and a triplet of NH2 group at 25 °C. At the same conditions the acylthioureas exhibit a doublet of NH group, the NH2 group signal being split into a doublet of doublets with different coupling constants 1J(15N, H). The greater one of these coupling constants is due to the s-trans proton with respect to the sulfur atom of the thiourea.

13C and 1H NMR spectra of all methyl O-benzoyl-β-D-xylopyranosides. nonadditivity of acylation effects on 13C chemical shifts in deutoriochloroform solutions

1983 ◽  
Vol 48 (3) ◽  
pp. 877-888 ◽  
Author(s):  
Eva Petráková ◽  
Jan Schraml
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Chemical Shifts ◽  
Coupling Constants ◽  
Conformational Heterogeneity ◽  
Additivity Rule ◽  
Homonuclear Decoupling ◽  
First Order ◽  
H Nmr ◽  
C Nmr

All methyl O-benzoyl-β-D-xylopyranosides have been prepared and their 1H and 13C NMR spectra measured in deuteriochloroform solutions. The 1H NMR spectra were analysed to the first order and assigned with the aid of homonuclear decoupling. The 13C chemical shifts were assigned through heteronuclear selective decouling experiments. Some of the 13C chemical shifts observed in di- and tri-O-benzoyl derivatives differ considerably from those calculated according to the direct additivity rule from the shifts in the mono derivatives. It is shown that the nonadditivity is due to a conformational heterogeneity of the series of investigated compounds dissolved in deuteriochloroform. The heterogeneity is evidenced by the vicinal 1H-1H coupling constants and by 13 chemical shifts of C(1) methoxyl carbon atoms.

Preparation and 1H NMR study of soluble alkoxy, alkyl and arylamido derivatives of sodium tetraamidoaluminate

1982 ◽  
Vol 47 (2) ◽  
pp. 384-391 ◽  
Author(s):  
Otomar Kříž ◽  
František Mareš ◽  
Bohuslav Čásenský
Keyword(s):  
1H Nmr ◽  
Aromatic Amines ◽  
Nmr Spectra ◽  
Pyridine Solution ◽  
Molecular Weights ◽  
H Nmr ◽  
Nmr Study ◽  
Derivatives Of

Sodium tetraamidoaluminate reacts with alcohols and aromatic amines under formation of sodium alkoxyimidoaluminates or amido(arylamido)aluminates, respectively. The corresponding sodium amido(alkylamido)aluminates were prepared from sodium tetraamidoaluminate and sodium tetrakis(alkylamido)aluminates in 1,2-dimethoxyethane or pyridine solution. 1H NMR spectra and in some cases also the cryoscopic molecular weights of the prepared compounds were measured.

scholarly journals Diagnostically analyzing 1H NMR spectra of sub-types in chaetoglobosins for dereplication

RSC Advances ◽  
2020 ◽  
Vol 10 (4) ◽  
pp. 1946-1955 ◽  
Author(s):  
Chen Lin ◽  
Jian-chun Qin ◽  
Yong-gang Zhang ◽  
Gang Ding
Keyword(s):  
Chemical Shift ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Diagnostic Information ◽  
1H Nmr Spectra ◽  
Coupling Constants ◽  
H Nmr

1H-NMR spectra provide abundant diagnostic information including chemical shift values, splitting patterns, coupling constants, and integrals.

1H NMR spectra and the conformation of 1,6 : 2,3- and 1,6 : 3,4-dianhydro-β-D-hexopyranoses and their derivatives

1979 ◽  
Vol 44 (6) ◽  
pp. 1965-1983 ◽  
Author(s):  
Miloš Buděšínský ◽  
Miloslav Černý ◽  
Tomáš Trnka ◽  
Soňa Vašíčková
Keyword(s):  
Hydrogen Bonds ◽  
1H Nmr ◽  
Torsion Angle ◽  
Nmr Spectra ◽  
Chemical Shifts ◽  
Point Of View ◽  
Coupling Constants ◽  
H Nmr ◽  
Vicinal Coupling Constants ◽  
Intramolecular Hydrogen

The 1H NMR spectra of 1,6 : 2,3- and 1,6 : 3,4-dianhydro-β-D-hexopyranoses and their acetyl-, trichloroacetylcarbamoyl- and 2- or 4-deoxy derivatives were measured in hexadeuteriodimethyl sulfoxide or deuteriochloroform. In these solvents dianhydro derivatives assume the half-chair conformations 5H0 or 1H0 which are not distinctly affected by the presence of substituents. The effects of substituents on the chemical shifts and the adjusted relation for the dependence of the vicinal coupling constants on the torsion angle are discussed from the point of view of conformation and the interactions of the oxirane ring with the oxygen O(5) and O(6) of the 1,6-anhydropyranose skeleton. Intramolecular hydrogen bonds in free dianhydrohexopyranoses were measured and identified in tetrachloromethane solution.

1H NMR Study of 3,5-Disubstituted 6-Oxo-1,6-dihydro-1,2,4-triazines

1995 ◽  
Vol 60 (2) ◽  
pp. 251-256
Author(s):  
Karel Nálepa ◽  
Aleš Halama ◽  
Taťjana Nevěčná ◽  
Vojtěch Bekárek
Keyword(s):  
Temperature Dependence ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Thermodynamic Characteristics ◽  
H Nmr ◽  
Nmr Study

1H NMR spectra have been measured of seven 3,5-disubstituted 6-oxo-1,6-dihydro-1,2,4-triazines, and tautomerism of these compounds has been evaluated in connection with the nature of substituents, medium, and temperature. The title compounds exist in their benzyl or benzylidene forms or as a mixture of both forms. Thermodynamic characteristics of the transition between the two forms have been determined from the temperature dependence of NMR spectra of three derivatives.

scholarly journals 1H-NMR study of some new acetyl dimethylbiphenyls: unambiguous signal assignment for the methyl groups

1997 ◽  
Vol 13 (2) ◽  
pp. 125-129 ◽  
Author(s):  
Fadhil S. Kamounah ◽  
Salam J. Titinchi
Keyword(s):  
1H Nmr ◽  
Structure Elucidation ◽  
Nmr Spectra ◽  
Methyl Groups ◽  
H Nmr ◽  
Signal Assignment ◽  
Nmr Study

The abundance1H-NMR spectra of some new mono- and diacetyl compounds derived from 2,2′-dimethyl-, 3,3′-dimethyl-, and 4,4′-dimethylbiphenyls were recorded. Unambiguous signal assignment of the methyl groups of the aromatic biphenyl rings were made for the structure elucidation.

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