In situ reactions of amines and amino alcohols and their application to structural assignment by 1H NMR spectroscopy

1980 ◽  
Vol 45 (10) ◽  
pp. 2784-2803 ◽  
Author(s):  
Miloš Buděšínský ◽  
Zdeněk Samek ◽  
Miloš Tichý
Keyword(s):  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
1H Nmr Spectroscopy ◽  
Amino Alcohols ◽  
Sample Tube ◽  
H Nmr ◽  
Structural Assignment ◽  
Trichloroacetyl Isocyanate ◽  
In Situ Reactions

The in situ reaction of amines with trichloroacetyl isocyanate (TAI) in the NMR sample tube was investigated as a tool in structural analysis by means of 1H NMR spectroscopy. Preferred conformations of the adducts were suggested which explain different behaviour of NH protons and the induced CH protons shifts. On the example of amino alcohols it was shown how to use the TAI method in combination with other in situ reactions (protonation, acetylation, trifluoroacetylation) for simultaneous differentiation between functional groups in polyfunctional molecules.

In situ reactions with trichloroacetyl isocyanate and their application to structural assignment of hydroxy compounds by 1H NMR spectroscopy. A general comment

1979 ◽  
Vol 44 (2) ◽  
pp. 558-588 ◽  
Author(s):  
Zdeněk Samek ◽  
Miloš Buděšínský
Keyword(s):  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Functional Groups ◽  
1H Nmr Spectroscopy ◽  
H Nmr ◽  
Structural Assignment ◽  
Trichloroacetyl Isocyanate ◽  
In Situ Reactions ◽  
Hydroxy Compounds

The application possibilities of the in situ reactions of trichloroacetyl isocyanate (TAI method) to structural assignment of alcohols by means of 1H NMR spectroscopy are critically evaluated. The possibilities of TAI acylations in various solvents are demonstrated and the reactivity of various functional groups, potentially complicating or extending the applications of TAI, is discussed. In addition to their use in structural analysis such reactions also can serve as model experiments for preparative purposes.

Conformational study on ribonucleoside O-phosphonylmethyl derivatives by 1H NMR spectroscopy

1985 ◽  
Vol 50 (8) ◽  
pp. 1899-1905 ◽  
Author(s):  
Milena Masojídková ◽  
Jaroslav Zajíček ◽  
Miloš Buděšínský ◽  
Ivan Rosenberg ◽  
Antonín Holý
Keyword(s):  
Nmr Spectroscopy ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Conformational Study ◽  
H Nmr ◽  
Conformational Properties

Conformational properties of ribonucleoside 5'-O-phosphonylmethyl derivatives have been determined by 1H NMR spectroscopy and compared with those of natural nucleosides and 5'-nucleotides.

The Origin of Molecular Mobility During Biomass Pyrolysis as Revealed by In situ 1H NMR Spectroscopy

ChemSusChem ◽  
2012 ◽  
Vol 5 (7) ◽  
pp. 1258-1265 ◽  
Author(s):  
Anthony Dufour ◽  
Miguel Castro-Diaz ◽  
Nicolas Brosse ◽  
Mohamed Bouroukba ◽  
Colin Snape
Keyword(s):  
Nmr Spectroscopy ◽  
1H Nmr ◽  
Molecular Mobility ◽  
1H Nmr Spectroscopy ◽  
Biomass Pyrolysis

Revisiting the iridacycle-catalyzed hydrosilylation of enolizable imines

2018 ◽  
Vol 8 (24) ◽  
pp. 6316-6329
Author(s):  
Jorge Pèrez-Miqueo ◽  
Virginia San Nacianceno ◽  
F. Borja Urquiola ◽  
Zoraida Freixa
Keyword(s):  
Nmr Spectroscopy ◽  
H Nmr

In situ1H NMR spectroscopy reveals a cascade mechanism for the hydrosilylation of enolizable imines catalyzed by iridium(iii) metallacycles.

scholarly journals Assessment of 1H NMR Spectroscopy for Specific Metabolite Fingerprinting of Angelica sinensis

2008 ◽  
Vol 3 (5) ◽  
pp. 1934578X0800300
Author(s):  
Dongmin Su ◽  
Jinglan Han ◽  
Shishan Yu ◽  
Hailin Qin
Keyword(s):  
Nmr Spectroscopy ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Authentic Sample ◽  
Angelica Sinensis ◽  
Metabolite Fingerprinting ◽  
H Nmr ◽  
Pure Compounds ◽  
Polar Extracts

The 1H NMR fingerprints of fractionated non-polar extracts (CSPD A) from the roots of Angelica sinensis of six different specimens were assigned by comparison with the 1H NMR spectra of the isolated pure compounds. The 1H NMR fingerprints showed exclusively characteristic resonance signals of the major constituents of the plant. The 1H NMR fingerprint established for an authentic sample of A. sinensis can be used for authenticating A. sinensis species.

Comparison of hydrogenolysis with thioacidolysis for lignin structural analysis

Holzforschung ◽  
2014 ◽  
Vol 68 (2) ◽  
pp. 151-155 ◽  
Author(s):  
Daniel J. van de Pas ◽  
Bernadette Nanayakkara ◽  
Ian D. Suckling ◽  
Kirk M. Torr
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Gas Chromatography ◽  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Magnetic Resonance ◽  
Gas Chromatography Mass Spectrometry ◽  
Aryl Ether ◽  
Chromatography Mass Spectrometry

Abstract Mild hydrogenolysis has been compared with thioacidolysis as a method for degrading lignins in situ and in isolated form before analysis by gas chromatography/mass spectrometry and quantitative 31P nuclear magnetic resonance (NMR) spectroscopy. Both degradation methods gave similar levels of β-aryl ether-linked phenylpropane units that were released as monomers. Degradation by hydrogenolysis generally gave lower levels of total phenylpropane units when analyzed by 31P NMR, especially in the case of lignins with high levels of condensed units. Overall, these results indicate that mild hydrogenolysis could offer an alternative to thioacidolysis for probing lignin structure.

Low-field 1H-NMR spectroscopy for compositional analysis of multicomponent polymer systems

The Analyst ◽  
2019 ◽  
Vol 144 (5) ◽  
pp. 1679-1686 ◽  
Author(s):  
Sneha B. Chakrapani ◽  
Michael J. Minkler ◽  
Bryan S. Beckingham
Keyword(s):  
Nmr Spectroscopy ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Compositional Analysis ◽  
Polymer Systems ◽  
H Nmr ◽  
Low Field ◽  
Multicomponent Polymer

A low-field, 60 MHz, 1H NMR spectrometer yields quantitatively comparable results to 400 MHz spectrometers for the compositional analysis of multicomponent polymer systems.

Sign in / Sign up

Export Citation Format

Share Document