Gradient-Enhanced Inverse-Detected NMR Techniquesfor Determination of 1H-15N Coupling Constants in 2,2-Dimethylpenta-3,4-dienal Derivatives

1997 ◽  
Vol 62 (11) ◽  
pp. 1747-1753 ◽  
Author(s):  
Radek Marek
Keyword(s):  
Double Bond ◽  
Chemical Shifts ◽  
Multiple Bond ◽  
Coupling Constants ◽  
Single Quantum ◽  
Nmr Techniques ◽  
Phase Sensitive ◽  
Heteronuclear Coupling

Determination of 15N chemical shifts and heteronuclear coupling constants of substituted 2,2-dimethylpenta-3,4-dienal hydrazones is presented. The chemical shifts were determined by gradient-enhanced inverse-detected NMR techniques and 1H-15N coupling constants were extracted from phase-sensitive gradient-enhanced single-quantum multiple bond correlation experiments. Stereospecific behaviour of the coupling constants 2J(1H,15N) and 1J(1H,13C) has been used to determine the configuration on a C=N double bond. The above-mentioned compounds exist predominantly as E isomers in deuteriochloroform.

Ultra high-resolution HSQC: application to the efficient and accurate measurement of heteronuclear coupling constants

2015 ◽  
Vol 51 (15) ◽  
pp. 3262-3265 ◽  
Author(s):  
Núria Marcó ◽  
André Fredi ◽  
Teodor Parella
Keyword(s):  
High Resolution ◽  
Coupling Constants ◽  
Rapid Acquisition ◽  
Enhanced Resolution ◽  
Nmr Techniques ◽  
Acquisition Strategy ◽  
Heteronuclear Coupling

A rapid acquisition strategy in terms of enhanced resolution per time unit for the simple and efficient determination of multiple coupling constants is proposed. The use of 13C spectral aliasing combined with pure shift NMR techniques allows accurate measurements of the magnitude and the sign from ultra high resolved 2D cross-peaks.

scholarly journals Accurate determination of one-bond heteronuclear coupling constants with “pure shift” broadband proton-decoupled CLIP/CLAP-HSQC experiments

2014 ◽  
Vol 239 ◽  
pp. 130-138 ◽  
Author(s):  
István Timári ◽  
Lukas Kaltschnee ◽  
Andreas Kolmer ◽  
Ralph W. Adams ◽  
Mathias Nilsson ◽  
...  
Keyword(s):  
Accurate Determination ◽  
Coupling Constants ◽  
Heteronuclear Coupling

Hétérobicycles oxygénés. Synthèse d'alkyl-3,6,8-trioxabicyclo[3.2.1]octanes et d'alkyl-3,7,9 et -4,7,9-trioxabicyclo[4.2.1]nonanes

1978 ◽  
Vol 56 (17) ◽  
pp. 2292-2300 ◽  
Author(s):  
Pierre Calinaud ◽  
Jacques Gelas
Keyword(s):  
Double Bond ◽  
Carbon Atom ◽  
Nmr Spectra ◽  
Membered Ring ◽  
Coupling Constants ◽  
Basic Medium ◽  
Main Interest ◽  
Proton Coupling ◽  
Geminal Proton

The cyclization in a basic medium of 2 (or 4)-chloroalkyl-4 (or 2) -hydroxyalkyl-1,3-dioxolanes leads to bicyclic acetals, the 3,6,8-trioxabicyclo[3.2.1]octanes, which are useful intermediates for synthesis, yielding notably functionalized 1,4-dioxanes. The nmr spectra of these heterobicyclics were studied. The geminal proton coupling constants permit oneto distinguish between five- and six-membered rings and the determination of couplings over several bonds (4J and 5J) yields information concerning the conformation of the model bicyclics.Two isomeric series of alkylated bicyclic acetals (3,7,9- and 4,7,9-trioxabicyclo[4.2.1]nonanes) are accessible by the following routes: (a) the intramolecular addition of a 4-hydroxy-alkyl group to the ethylenic double bond on the carbon atom a to C-2 in the 1,3-dioxolanes; (b) the dechlorohydration of 2-chloromethyl-4-hydroxyalkyl-1,3-dioxolanes; (c) the dehydration of dioxolane-diols. The main interest in these heterobicyclics is to prepare a seven-membered ring and to be able to prepare functionalized 1,4-dioxepanes. [Journal translation]

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