m-SuIfobenzaldehyde in FD&C Violet No. 1

1969 ◽  
Vol 52 (3) ◽  
pp. 622-626
Author(s):  
Daniel M Marmion
Keyword(s):  
Nmr Spectra ◽  
Retention Volume ◽  
Chromatographic Retention ◽  
Ir And Nmr Spectra ◽  
Nmr Data ◽  
Unknown Substance ◽  
Dimethylaminobenzoic Acid

Abstract An unknown substance present in FD&C Violet No. 1 has been identified as m-sulfobenzaldehyde containing a small amount of p-sulfobenzaldehyde. Identification is based on the coincidence of the UV, IR, and NMR spectra of the unknown, as well as the chromatographic retention volume of the unknown, with those of m-sulfobenzaldehyde. The presence of some p-sulfobenzaldehyde is shown by NMR data. A method is also described for the determination of m-sulfobenzaldehyde and the estimation of p-dimethylaminobenzaldehyde, p-dimethylaminobenzoic acid, and ethylbenzylanilinesulfonic acid.

Determination of the Enantiomeric Excess of Horner Phosphines by 13C NMR Spectroscopy. A 13C and 31P NMR Study of the Diastereomeric Complexes Formed with [η3-(+)(1R,5R )-Pinenyl]nickel Bromide Dimer

1986 ◽  
Vol 41 (1) ◽  
pp. 85-88 ◽  
Author(s):  
Richard Mynott ◽  
Wolf Jürgen Richter ◽  
Günther Wilke
Keyword(s):  
Nmr Spectra ◽  
31P Nmr ◽  
Enantiomeric Excess ◽  
13C Nmr Spectroscopy ◽  
Nmr Data ◽  
Nmr Study ◽  
Diastereomeric Complexes ◽  
13C And 31P Nmr ◽  
Good Agreement

The 13C and 31P NMR data of the Horner phosphines PRR′R″ [R = Me. R′ = t-Bu, R'″ = Ph (2) or i-Pr (4)] and their diastereomeric 1:1 adducts with [η3-(+)(1 R, 5 R)-pinenyI]nickel bromide dimer (3) and (5), respectively, are reported. It is shown that the optical purities of the phosphines can be deduced easily from the NMR spectra. Not only are these values in very good agreement with those obtained from optical rotatory data but they are also obtained much more conveniently.

Offene und geschlossene P-funktionalisierte Diferriophosphonium-Salze des Typs [ { CpFe(CO)2}2P(Ph)R]+ X⁻ bzw. [ {μ-CO(CpFeCO)2} P(Ph)R]+ X⁻ / Open and Closed P-Functionalized Diferriophosphonium Salts of the Type [{CpFe(CO)2}2P(Ph)R]+ X⁻ and [{ μ-CO(CpFeCO)2}P(Ph)R]+ X⁻

1993 ◽  
Vol 48 (6) ◽  
pp. 705-712 ◽  
Author(s):  
Christian Klasen ◽  
Guido Effinger ◽  
Siegbert Schmid ◽  
Ingo-Peter Lorenz
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Nmr Spectra ◽  
Crystal Structure Determination ◽  
Ir And Nmr Spectra ◽  
Deprotonation Reaction ◽  
Alkylating Reagents

The reaction of Ph(R)PSiMe3 with an excess of CpFe(CO)2Cl results in the elimination of Me3SiCl to give the open diferriophosphonium halides [{CpFe(CO)2}2P(Ph)R]Cl (R = H, Ph, CH2SiMe3, Me) (1 a—d). The deprotonation reaction of 1 a with KOBut at —78°C results in the formation of the unstable diferriophosphane {CpFe(CO)2}2PPh (3), which reacts with alkylating reagents RX (R = Me, CH2Ph, CH2COOEt; X = Cl, I) to give the P-functionalized diferriophosphonium halides [{CpFe(CO)2}2P(Ph)R]X (1 d’—f). The light-sensitive compounds 1b—f are found to eliminate readily a CO ligand upon photolysis to give the corresponding closed P-functionalized diferriophosphonium salts [{µ-CO(CpFeCO)2}P(Ph)R]X (2b—f) with a bridging CO ligand and a Fe— Fe bond. The mass, IR and NMR spectra of 1, 2 and the results of a crystal structure determination of [{μ-CO(CpFeCO)2}PPh2]BPh4 (2b’) are reported and discussed.

IR, 31P-, 55 Mn-und 185,187 Re-NMR spektroskopische Untersuchungen an einigen Carbonylmangan-und -rhenium-Komplexen/IR, 31P, 55Mn and 185,187Re NMR Spectroscopic Investigations of Some Carbonylmanganese and -rhenium Complexes

1981 ◽  
Vol 36 (1) ◽  
pp. 20-26 ◽  
Author(s):  
Ahmet Keçeci ◽  
Dieter Rehder
Keyword(s):  
Spectroscopic Data ◽  
Nmr Spectra ◽  
Rhenium Complexes ◽  
Ir And Nmr Spectra ◽  
Π Interactions ◽  
Spectroscopic Investigations ◽  
Ligand System ◽  
Nmr Data ◽  
Rhenium Compound ◽  
Metal Ligand

Abstract The IR and NMR spectra of the complexes [M(CO)6]Cl · HCl (M = Mn: 1, M = Re: 2), M(C0)5C02Et (M = Mn: 3, M = Re: 4), [Mn(CO)5PR3][PF6] (5; PR3 = PPh(OPh)2: a, P(n-Pr)3: b, PHPh2: c, PPh(NEt2)2: d, P(p-C6H4F)3: e), [Re(CO)5PHPh2][PF6] (6 c), Mn2(CO)8(PR3)2 (7) and Re2(CO)8(PHPh2)2 (8c) are discussed in the context of σ-and π-interactions in the metal-ligand system and compared with 51V NMR data of the analogous isoelectronic and isostructural carbonylvanadates (-I). On the basis of these results, the phosphines are arranged in the order of decreasing integral ligand strength according to a>b>c>d. The 55Mn shielding of 5 is greater than that of 1, which is explained by strong σ-interactions and correspondingly large e-a1* splitting dominating the paramagnetic deshielding term in the pseudooctahedral complexes of type 5. The only rhenium compound accessible to NMR is 2, for which the 185 Re and 187 Re resonances were obtained. 31P coordination shifts are positive for all complexes. Spectroscopic data for 7c show that this complex presumably has the structure (CO)5Mn-Mn(CO)3(PHPh2)2, contrasting 7a, 7b, 7d and 7e (local D4d symmetry).

MONOREG – an expert system for structural elucidation of monoterpenes

2001 ◽  
Vol 79 (12) ◽  
pp. 1915-1925 ◽  
Author(s):  
Marcelo J Ferreira ◽  
Gilberto V Rodrigues ◽  
Vicente P Emerenciano
Keyword(s):  
Expert System ◽  
Nmr Spectra ◽  
Structural Elucidation ◽  
Structural Determination ◽  
Systematic Data ◽  
Data Analyses ◽  
Nmr Data ◽  
Living Organisms ◽  
C Nmr

This paper describes a new expert system denominated MONOREG for structural determination of monoterpenes. This system is composed of five programs capable of performing 13C NMR spectra data analyses and analyses of systematic data from living organisms. At the end of this procedure, it shows the likely skeletons of the compound in question as well as the substructures compatible with the 13C NMR data. The system was tested on the skeleton elucidation of 40 monoterpenes from a wide variety of structure types and exhibited excellent results in the skeleton prediction process.

NMR Determination of the Structure of Peracetylated Icariside B2 from Veratrum Lobelianum BERNH.

1995 ◽  
Vol 60 (8) ◽  
pp. 1380-1385 ◽  
Author(s):  
Václav Suchý ◽  
Miloš Buděšínský ◽  
Karel Ubik ◽  
Daniel Grančai ◽  
Vlasta Földešiová
Keyword(s):  
Detailed Analysis ◽  
Nmr Spectra ◽  
Aerial Part ◽  
C Nmr

rel(1S,4S,5R)-3,3,5-Trimethyl-4-[( 1E)-3-oxo-1-butenyl]-4,5-epoxy-cyclohexyl-O-β-D-glucopyranoside (I) was isolated from the aerial part of Veratrum lobelianum BERNH. The structure was derived mainly from detailed analysis of 1H and 13C NMR spectra of its acetylated derivative II. Compound I has been already reported under the name icariside B2in Epimedium grandiflorum MORR. var. thunbergianum (MIQ.) NAKAI.

scholarly journals Structural characteristics of plant cell wall elucidated by solution-state 2D NMR spectroscopy with an optimized procedure

2020 ◽  
Vol 9 (1) ◽  
pp. 650-663
Author(s):  
Wanwan Wang ◽  
Jibao Cai ◽  
Zhenyu Xu ◽  
Yi Zhang ◽  
Fanchao Niu ◽  
...  
Keyword(s):  
Cell Wall ◽  
Quantum Coherence ◽  
Nmr Spectra ◽  
Plant Cell Wall ◽  
Milling Time ◽  
Structural Characteristics ◽  
2D Nmr ◽  
2D Nmr Spectroscopy ◽  
Complete Representation

AbstractA method was developed for rapid qualitative determination of lignocellulose in the tobacco cell wall by utilizing 2D heteronuclear single quantum coherence NMR spectra (2D HSQC NMR). Traditional methods for analyzing the structure of lignocellulose involve many steps of separation and extraction, which is labor-intensive. In this work, the whole cell wall was milled and dissolved in deuterium solvent. The solvent dimethylsulfoxide (DMSO-d6) containing hexamethylphosphoramide (HMPA-d18) enhanced swelling of the sample and gave high-resolution spectra. The tobacco samples are ball milled at different ball milling times, and the state of the particles is observed through an electron microscope, and then the probability of the particles being less than 5 µm is counted. Through the comparison of the abundance and integration of the peak signals in the spectra under different transmittances, it was determined that when the milling time was 6 h, the quality of the NMR spectra was the best. The optimum conditions of characterizing tobacco structure were DMSO-d6/HMPA-d18 solution and 6 h milling time. Under these conditions, complete representation of the structure of lignocellulose and simplified process could be achieved.

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