scholarly journals Determination of molar ratio of primary secondary and tertiary amines in polymers by applying derivatization and NMR spectroscopy

2016 ◽  
Vol 56 ◽  
pp. 174-179 ◽  
Author(s):  
Qing Liu ◽  
Marcel Zhu

1980 ◽  
Vol 58 (11) ◽  
pp. 1069-1074 ◽  
Author(s):  
Harold J. Jennings ◽  
Karl-Gunnar Rosell ◽  
Dennis J. Carlo

The structure of the Pneumococcus type-19 (19F) capsular polysaccharide has been reinvestigated using nmr spectroscopy. It is composed of residues of 2-acetamido-2-deoxy-D-mannose, D-glucose, L-rhamnose, and phosphate in the molar ratio of 1:1:1:1. The polysaccharide is linear and is composed of the above components in a repeating unit of the following structure:→ 4)-β-D-ManNAcp-(1 → 4)-α-D-Glcp-(1→ 2)-α-L-Rhap-(1-PO4−)→.



2020 ◽  
Author(s):  
Ashraf Ismail ◽  
Sanaz Molaye Moghaddam ◽  
Jean-Pierre MetabanzoulouSarya Aziz ◽  
Jacqueline Sedman ◽  
Mazen Bahadi


1982 ◽  
Vol 47 (7) ◽  
pp. 1973-1978 ◽  
Author(s):  
Jiří Karhan ◽  
Zbyněk Ksandr ◽  
Jiřina Vlková ◽  
Věra Špatná

The determination of alcohols by 19F NMR spectroscopy making use of their reaction with hexafluoroacetone giving rise to hemiacetals was studied on butanols. The calibration curve method and the internal standard method were used and the results were mutually compared. The effects of some experimental conditions, viz. the sample preparation procedure, concentration, spectrometer setting, and electronic integration, were investigated; the conditions, particularly the concentrations, proved to have a statistically significant effect on the results of determination. For the internal standard method, the standard deviation was 0.061 in the concentration region 0.032-0.74 mol l-1. The method was applied to a determination of alcohols in the distillation residue from an oxo synthesis.



Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 2039
Author(s):  
Gamal A. E. Mostafa ◽  
Ahmed Bakheit ◽  
Najla AlMasoud ◽  
Haitham AlRabiah

The reactions of ketotifen fumarate (KT) with 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) and 7,7,8,8-tetracyanoquinodimethane (TCNQ) as π acceptors to form charge transfer (CT) complexes were evaluated in this study. Experimental and theoretical approaches, including density function theory (DFT), were used to obtain the comprehensive, reliable, and accurate structure elucidation of the developed CT complexes. The CT complexes (KT-DDQ and KT-TCNQ) were monitored at 485 and 843 nm, respectively, and the calibration curve ranged from 10 to 100 ppm for KT-DDQ and 2.5 to 40 ppm for KT-TCNQ. The spectrophotometric methods were validated for the determination of KT, and the stability of the CT complexes was assessed by studying the corresponding spectroscopic physical parameters. The molar ratio of KT:DDQ and KT:TCNQ was estimated at 1:1 using Job’s method, which was compatible with the results obtained using the Benesi–Hildebrand equation. Using these complexes, the quantitative determination of KT in its dosage form was successful.



Author(s):  
Xuming Sha ◽  
Shaodong Chen ◽  
Xiaojing Zheng ◽  
Xin Ye ◽  
Hailu Zhang ◽  
...  


Tetrahedron ◽  
2020 ◽  
pp. 131827
Author(s):  
Sándor Nagy ◽  
Áron Szigetvári ◽  
Viktor Ilkei ◽  
Balázs Krámos ◽  
Zoltán Béni ◽  
...  


1989 ◽  
Vol 4 (7) ◽  
pp. 175-179 ◽  
Author(s):  
Barbro Andersson ◽  
Kurt Andersson
Keyword(s):  


1993 ◽  
Vol 48 (1) ◽  
pp. 58-67 ◽  
Author(s):  
Joseph Grobe ◽  
Duc Le Van ◽  
Gudrun Lange

The course of the reactions o f fluorophosphaalkenes F3CP = C (F)OR [R = Me (1), Et (2)] with methanol or ethanol strongly depends on the experimental conditions. Thus at 70 °C a mixture of the 2-phosphapropionic acid ester F3CP (H )CO2R [R = Me (3), Et (4)] and trifluoromethylphosphane H2PCF3 is formed [molar ratio: 3 or 4 /H2 CF3 ≈1/1]. If the precursors F3CP (H )CO2R [R = Me (3), Et) are used as starting materials, the reaction with ROH under the same conditions affords 3 and 4, respectively, (90 to 95% yield) with only traces of H2PCF 3. In the presence o f iPr2NH these precursors react with R′OH to give the novel trifluoromethylphosphaalkenes F3CP = C (OR )OR [R /R′: Me/Me (6); E t/E t (7); Me/Et (8)]. With Et2NH , 3 undergoes an addition/elimination process yielding the interesting push/pull system Et2N(F)C = P-CO2Me (5). 1 and 2 react with primary amines R′NH2 (R′= tBu, Me) with stereoselective formation of the fairly labile phosphaalkenes F3CP = C(OR)NHR′ [R /R′: Me/tBu (9), Et/tBu(10), Me/Me (11)] with trans-positions for CF3 and NHR′.The new compounds 3 -11 were characterized by spectroscopic investigations (1H , 19F, 31P, 13C NMR ; IR, MS) and determination of M+ or typical fragment ions [M+ -OR ] by high resolution mass spectrometry.



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