Complete Assignment of the 1H and 13C NMR Spectra of Carthamin Potassium Salt Isolated from Carthamus Tinctorius L.

Complete Assignment ◽

Pure Product ◽

Atomic Adsorption Spectroscopy ◽

Nmr Signals ◽

C Nmr

Carthamin potassium salt isolated from Carthamus tinctorius L. was purified by an improved traditional Japanese method, without using column chromatography. The 1H and 13C nuclear magnetic resonance (NMR) signals of the pure product were fully assigned using one- and two-dimensional NMR spectroscopy, while the high purity of the potassium salt and deprotonation at the 3’ position of carthamin were confirmed by atomic adsorption spectroscopy and nano-electrospray ionization mass spectrometry.

Complete Assignment of the 1H and 13C NMR Spectra of Carthamin Potassium Salt Isolated from Carthamus tinctorius L.

Molecules ◽

10.3390/molecules26164953 ◽

2021 ◽

Vol 26 (16) ◽

pp. 4953

Author(s):

Maiko Sasaki ◽

Keiko Takahashi

Keyword(s):

Potassium Salt ◽

Nmr Spectra ◽

Carthamus Tinctorius ◽

Ionization Mass ◽

1H And 13C Nmr ◽

Complete Assignment ◽

Pure Product ◽

Atomic Adsorption Spectroscopy ◽

Nmr Signals

Carthamin potassium salt isolated from Carthamus tinctorius L. was purified by an improved traditional Japanese method, without using column chromatography. The 1H and 13C nuclear magnetic resonance (NMR) signals of the pure product were fully assigned using one- and two-dimensional NMR spectroscopy, while the high purity of the potassium salt and deprotonation at the 3′ position of carthamin were confirmed by atomic adsorption spectroscopy and nano-electrospray ionization mass spectrometry.

Qinghaosu: 1H and 13C nuclear magnetic resonance spectral assignments and luminescence

10.1139/v85-508 ◽

1985 ◽

Vol 63 (11) ◽

pp. 3070-3074 ◽

Cited By ~ 17

Author(s):

Wang Zhongshan ◽

Thomas T. Nakashima ◽

Karl R. Kopecky ◽

José Molina

Keyword(s):

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Complete Assignment ◽

Methoxide Ion ◽

Nmr Signals ◽

Bright Luminescence ◽

C Nmr ◽

Nuclear Magnetic

The complete assignment of the 1H and 13C nmr signals for Qinghaosu 1 has been made. Treatment of 1 with methoxide ion at 80 °C results in bright luminescence when carried out in the presence of fluorescers. Several products are formed when methanol is present, but in toluene only one product is formed when methanol-free methoxide is used. Its structure is tentatively assigned as 1-(1-methoxycarbonylethyl)-2,6-dimethyl-2-hydroxybicyclo[3.3.1]nonan-9-one.

Carbon-13 and nitrogen-14 NMR spectra of 1-(substituted phenyl)pyridinium salts

Collection of Czechoslovak Chemical Communications ◽

10.1135/cccc19802766 ◽

1980 ◽

Vol 45 (10) ◽

pp. 2766-2771 ◽

Cited By ~ 8

Author(s):

Antonín Lyčka

Keyword(s):

Heavy Water ◽

Nmr Spectra ◽

Chemical Shifts ◽

Coupling Constants ◽

Pyridinium Salts ◽

Nmr Signals ◽

C Nmr

The 13C and 14N NMR spectra of 1M solutions of 1-(substituted phenyl)pyridinium salts (4-CH3, 4-OCH3, H, 4-Cl, 4-Br, 4-I, 3-NO2, 4-NO2, 2,4-(NO2)2 (the 13C NMR only)) have been measured in heavy water at 30 °C. The 13C and 14N chemical shifts, the 1J(CH) coupling constants, some 3J(CH) coupling constants, and values of half-widths Δ 1/2 of the 14N NMR signals are given. The 13C chemical shifts of C(4) correlate with the σ0 constants (δC(4) = (1.79 ± 0.097) σ0 + (147.67 ± 0.041)), whereas no correlation of the nitrogen chemical shifts with the σ constants has been found. The half-widths Δ 1/2 correlate with the σ0 constants (Δ 1/2 = (76.2 ± 4.9) σ0 + (106.4 ± 2.2)) except for 1-phenylpyridinium chloride.

E-Homolupane Derivatives Substituted in Position 17 and 22a. 1H NMR, 13C NMR and IR Spectra

Collection of Czechoslovak Chemical Communications ◽

10.1135/cccc19950619 ◽

1995 ◽

Vol 60 (4) ◽

pp. 619-635 ◽

Cited By ~ 1

Author(s):

Václav Křeček ◽

Stanislav Hilgard ◽

Miloš Buděšínský ◽

Alois Vystrčil

Keyword(s):

Nmr Spectra ◽

2D Nmr ◽

Coupling Constants ◽

Side Chain ◽

Oxidation Reactions ◽

H Nmr ◽

Complete Assignment ◽

Nmr Techniques ◽

Intramolecular Association ◽

C Nmr

A series of derivatives with various oxygen functionalities in positions 17,22a or 19,20 was prepared from diene I and olefin XVI by addition and oxidation reactions. The structure of the obtained compounds was confirmed by 1H NMR, 13C NMR and IR spectroscopy. The kind of intramolecular association of the 17α-hydroxy group was studied in connection with modification of the side chain and substitution in position 22a. Complete assignment of the hydrogen signals and most of the coupling constants was accomplished using a combination of 1D and 2D NMR techniques. The 1H and 13C NMR spectra are discussed.

Propionate stimulates pyruvate oxidation in the presence of acetate

AJP Heart and Circulatory Physiology ◽

10.1152/ajpheart.00407.2014 ◽

2014 ◽

Vol 307 (8) ◽

pp. H1134-H1141 ◽

Cited By ~ 14

Author(s):

Colin Purmal ◽

Blanka Kucejova ◽

A. Dean Sherry ◽

Shawn C. Burgess ◽

Craig. R. Malloy ◽

...

Keyword(s):

Pyruvate Dehydrogenase ◽

Energy Production ◽

Nmr Spectra ◽

Heart Tissue ◽

Viable Myocardium ◽

Normal Heart ◽

Alternative Substrate ◽

Isotopomer Analysis ◽

Nmr Signals ◽

C Nmr

Flux through pyruvate dehydrogenase (PDH) in the heart may be reduced by various forms of injury to the myocardium, or by oxidation of alternative substrates in normal heart tissue. It is important to distinguish these two mechanisms because imaging of flux through PDH based on the appearance of hyperpolarized (HP) [13C]bicarbonate derived from HP [1-13C]pyruvate has been proposed as a method for identifying viable myocardium. The efficacy of propionate for increasing PDH flux in the setting of PDH inhibition by an alternative substrate was studied using isotopomer analysis paired with exams using HP [1-13C]pyruvate. Hearts from C57/bl6 mice were supplied with acetate (2 mM) and glucose (8.25 mM). 13C NMR spectra were acquired in a cryogenically cooled probe at 14.1 Tesla. After addition of hyperpolarized [1-13C]pyruvate, 13C NMR signals from lactate, alanine, malate, and aspartate were easily detected, in addition to small signals from bicarbonate and CO2. The addition of propionate (2 mM) increased appearance of HP [13C]bicarbonate >30-fold without change in O2 consumption. Isotopomer analysis of extracts from the freeze-clamped hearts indicated that acetate was the preferred substrate for energy production, glucose contribution to energy production was minimal, and anaplerosis was stimulated in the presence of propionate. Under conditions where production of acetyl-CoA is dominated by the availability of an alternative substrate, acetate, propionate markedly stimulated PDH flux as detected by the appearance of hyperpolarized [13C]bicarbonate from metabolism of hyperpolarized [1-13C]pyruvate.

13C nuclear magnetic resonance and Raman investigations of aqueous carbon dioxide systems

10.1139/v82-149 ◽

1982 ◽

Vol 60 (8) ◽

pp. 1000-1006 ◽

Cited By ~ 33

Author(s):

Theresa M. Abbott ◽

Gerald W. Buchanan ◽

Peeter Kruus ◽

Keith C. Lee

Keyword(s):

Carbon Dioxide ◽

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Linear Relationship ◽

Nmr Spectra ◽

Chemical Shifts ◽

Carbonate Ion ◽

Wide Range ◽

C Nmr

13C-nmr spectra of carbon dioxide in water are reported for a wide range in pH. Chemical shifts were determined for the following species: CO2(g), CO2(aq), HCO3−(aq), CO32−(aq). A linear relationship was found between the shift of the 13C line and the fraction of carbonate ion calculated to be present, as well as between the ratio of the area under the 1067 cm−1 (carbonate) Raman peak to the sum of the area under the 1067 cm−1 and 1017 cm−1 (bicarbonate) peaks and the fraction carbonate.

Electronic structure of low-spin six-coordinate iron(III) meso-tetrapropylchlorin complexes

Journal of Porphyrins and Phthalocyanines ◽

10.1142/s1088424614500576 ◽

2014 ◽

Vol 18 (08n09) ◽

pp. 778-791 ◽

Cited By ~ 2

Author(s):

Akira Ikezaki ◽

Jyunpei Ono ◽

Yoshiki Ohgo ◽

Mari Fukagawa ◽

Takahisa Ikeue ◽

...

Keyword(s):

Electronic Structure ◽

Ground State ◽

Nmr Spectra ◽

Spectroscopic Properties ◽

H Nmr ◽

Axial Ligands ◽

Splitting Parameter ◽

Nmr Signals ◽

Electronic Ground ◽

C Nmr

Low-spin iron(III) tetrapropylchlorins [ Fe ( T n PrC ) L 2]± (L = HIm, 1-MeIm, DMAP, CN-, 4-CNPy, tBuNC) adopt the dxy-type ground state regardless of the nature of axial ligands. Among the complexes examined, [ Fe ( T n PrC )( t BuNC )2]+ has shown quite unique spectroscopic properties as described below. (1) 1 H NMR signals were extremely broad as compared with those of other complexes. In particular, 5,20- CH 2(α) signal was too broad to detect. (2) No signals except C γ were observed in 13 C NMR spectra. (3) Tetragonal splitting parameter (|Δ|) estimated by the EPR g values at 4.2 K reached as much as 12.4 λ, which is the largest |Δ| value among all the low-spin iron(III) porphyrins and porphyrinoids reported previously. On the basis of these results, we have concluded that [ Fe ( T n PrC )( t BuNC )2]+ adopts the low-spin iron(III) with (dxz, dyz)4(dxy)1 electronic ground state at 4.2–30 K where the EPR spectra are taken, while it should be expressed as the low-spin Fe ( II ) chlorin π-radical cation [ Fe II ( T n PrC .)( t BuNC )2]+ at ambient temperature where the NMR spectra are taken.

On the chemistry and high field nuclear magnetic resonance spectroscopy of rapamycin

10.1139/v80-090 ◽

1980 ◽

Vol 58 (6) ◽

pp. 579-590 ◽

Cited By ~ 91

Author(s):

John A. Findlay ◽

Lajos Radics

Keyword(s):

High Field ◽

Nmr Spectra ◽

Resonance Spectroscopy ◽

X Ray ◽

Conformational Isomers ◽

H Nmr ◽

Neutral Compounds ◽

Complete Assignment ◽

Hydrolysis Of ◽

C Nmr

Base catalysed hydrolysis of rapamycin (C51H79NO13) affords six neutral compounds identified by chemical and spectroscopic means as 2a, 3b, 3d, 5, 2,4-dimethylphenol, and L(−)-piperidine-2-carboxylic acid 6, and whose generation has been plausibly rationalized. These findings as well as detailed analyses of 13C nmr and 1H nmr spectra provide independent corroboration of the X-ray derived rapamycin crystal structure 1. Structurally homogeneous in the solid state, rapamycin is found to occur in solutions as a mixture of two conformational isomers (approximately 4:1). Through nearly complete assignment of the high field 1H (400 MHz) and 13C (100.6 MHz) nmr spectra, the isomerism is shown to be associated with trans–cis rotation of an amidic bond within the 31-membered macrolide ring. The predominant form corresponds to the conformer portrayed by X-ray analysis.

13C nuclear magnetic resonance studies. 58. 13C spectra of a variety of bicyclo[2.2.2]octane derivatives. Further definition of the deshielding δ effect

10.1139/v76-133 ◽

1976 ◽

Vol 54 (6) ◽

pp. 917-925 ◽

Cited By ~ 50

Author(s):

J. B. Stothers ◽

C. T. Tan

Keyword(s):

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Nmr Spectra ◽

Magnetic Resonance Studies ◽

Definition Of ◽

C Nmr ◽

Nuclear Magnetic

The 13C nmr spectra of 35 bicyclo[2.2.2]octane and -octene derivatives have been determined to extend our examinations of the effects of stereochemistry on the shieldings of closely neighboring carbons. This series includes a variety of methyl substituted bicyclooctanols and -octenols as well as the corresponding hydrocarbons and some bicyclooctanones. With the bicyclo[2.2.2]octane skeleton it is possible to examine an array of systems having substituents separated by three and four bonds in a variety of orientations. The interactions, termed γ and δ effects, respectively, produce distinctive shielding variations which are useful for stereochemical elucidations. Particularly interesting are the pronounced shifts observed for the carbons bearing closely neighboring substituents. Characteristically, for vicinal substituents, these carbons are shielded while for syn-axial δ interactions, these carbons are deshielded by as much as 8.6 ppm. The results are compared with the trends found in other sterically crowded Systems.

13C nuclear magnetic resonance studies. 61. The effect of solute–solvent association on internal rotation in substituted benzaldehydes

10.1139/v76-466 ◽

1976 ◽

Vol 54 (20) ◽

pp. 3267-3271 ◽

Cited By ~ 7

Author(s):

R. E. Klinck ◽

J. B. Stothers

Keyword(s):

Steric Effect ◽

Methylene Chloride ◽

Activation Parameters ◽

Formyl Group ◽

Magnetic Resonance Studies ◽

Group Rotation ◽

Substituted Benzaldehydes ◽

Nmr Signals ◽

C Nmr

Complete lineshape analyses of the 13C nmr signals of the ortho and meta carbons have been carried out for two p-substituted benzaldehydes in methylene chloride-d2 and toluene-d8 solutions over a wide temperature range. The activation parameters have been determined for the formyl group rotation and large negative values are found for ΔS≠ when the latter solvent is used. These results suggest that solute–solvent association has a steric effect on the transition state.