scholarly journals Efficient Synthesis and Spectroscopic Characterization of Biologically Relevant Pregnane Derivatives, and its Glycoside

2020 ◽  
Vol 01 ◽  
Author(s):  
Arun Sethi ◽  
Ranvijay Pratap Singh ◽  
Akriti Bhatia ◽  
Priyanka Yadav

Objective:: In present research article, we synthesized novel pregnane derivatives from 16-dehydropregnenolone acetate (1) which has been obtained by the degradation of naturally occurring plant product-diosgenin. The oxime esters, 3β-acetoxy-pregn-5,16-diene, 20-one O-(2-(6-methoxynaphthalene-2yl) propionyl) oxime (5) and 3β-hydroxy-pregn-5, 16-diene, 20-one O-(2-(4-isobutyl phenyl) propionyl) oxime (6) have been synthesized by reaction of 3β-acetoxy-5,16-pregna-dien-20-oxime (3) with NSAIDs Ibuprofen and naproxen respectively. Methods:: The epoxide derivative 3β-hydroxy-16α, 17α-epoxypregn-5-ene-20-one (4) was opened by BF3.Et2O and yielding product 3,16-di-hydroxy pregn-5-ene-20-one (7) and 3,16,17-tri-hydroxy pregn-5-ene-20-one (8), both the synthesized compounds undergoes esterification with Ibuprofen afforded 3,16-di-(2-(4-isobutyl phenyl) propionoxy) pregn-5-ene-20-one (9) and 3,16-di-(2-(4-isobutyl phenyl) propionoxy) 17-hydroxy pregn-5-ene-20-one (10) respectively. Results and Conclusion:: A one novel pregnane glycoside 3β-[2′,3′,4′,6′-tetra-O-acetyl-β-D-glucopyranosyl]-Oxy-20β-hy-droxy-16α-methoxy-pregn-5-ene (15) has also been synthesized from 3β, 20β-dihydroxy-16α-methoxy-pregn-5-ene (12). After the synthesis all the compounds have been characterized by modern spectroscopic techniques.

2020 ◽  
Vol 45 (5) ◽  
Author(s):  
V.O. Uduah ◽  
J.J. Gongden ◽  
M.L. Kagoro ◽  
K.K. Gurumyen ◽  
Y.N. Lohdip ◽  
...  

This work presents a dry synthesis of Iron (III) complex with urea isolated from human urine and Fe (III) obtained from iron rust particles. Iron (III), PI (Purified iron rust), was isolated from iron rust in 10% hydrochloric acid, HCl and distilled water respectively. The complex was synthesized via dry-synthesis method using the melted urea as reaction medium. The isolated Fe (III) was characterized by elemental analysis which was done using XRF Cu-Zn method. The complex was prepared in a 1:4 metal to ligand (M-L) ratio. The stoichiometry of reaction indicate a 1:3 ratio of M-L (Fe-U). The complex was characterized by FT-IR, UV-vis, XRF and XRD spectroscopic techniques. The Fe (III) isolate and Fe-U complex shows percentage yields of 35.7% and ~92% respectively. The elemental and oxide composition of Fe and Fe2O3 (i.e., PI) were 40.387% and 57.753% respectively. The results obtained from the characterization of the iron-urea complex, IUC, indicate FT-IR result as symmetric and asymmetric frequencies with peaks of a combination band of Vs (NH) and Vas (NH), C=O and V (C-N) all stretched, XRD showed the crystal to be amorphous. The elemental and oxide composition of the Fe and Fe2O3 in IUC were 40.007 and 44.201 respectively. The results obtained revealed that useful complexes can be synthesized easily from waste materials, such as urine and iron rust particles, which complement Green chemistry.


Polymers ◽  
2019 ◽  
Vol 11 (9) ◽  
pp. 1498 ◽  
Author(s):  
Abdul Hafeez ◽  
Zareen Akhter ◽  
John F. Gallagher ◽  
Nawazish Ali Khan ◽  
Asghari Gul ◽  
...  

Bis-aldehyde monomers 4-(4′-formyl-phenoxy)benzaldehyde (3a), 3-methoxy-4-(4′-formyl-phenoxy)benzaldehyde (3b), and 3-ethoxy-4-(4′-formyl-phenoxy)benzaldehyde (3c) were synthesized by etherification of 4-fluorobenzaldehyde (1) with 4-hydroxybenzaldehyde (2a), 3-methoxy-4-hydroxybenzaldehyde (2b), and 3-ethoxy-4-hydroxybenzaldehyde (2c), respectively. Each monomer was polymerized with p-phenylenediamine and 4,4′-diaminodiphenyl ether to yield six poly(azomethine)s. Single crystal X-ray diffraction structures of 3b and 3c were determined. The structural characterization of the monomers and poly(azomethine)s was performed by FT-IR and NMR spectroscopic techniques and elemental analysis. Physicochemical properties of polymers were investigated by powder X-ray diffraction, thermogravimetric analysis (TGA), viscometry, UV–vis, spectroscopy and photoluminescence. These polymers were subjected to electrical conductivity measurements by the four-probe method, and their conductivities were found to be in the range 4.0 × 10−5 to 6.4 × 10−5 Scm−1, which was significantly higher than the values reported so far.


Author(s):  
Marta Siczek ◽  
Marcin Zawadzki ◽  
Miłosz Siczek ◽  
Agnieszka Chłopaś-Konowałek ◽  
Paweł Szpot

Abstract Purpose The aim of the study was to present the spectroscopic characteristics and crystal structure of the etazene—a benzimidazole opioid, which appeared on the illegal drug market in Poland in the last weeks. Methods The title compound was analyzed by X-ray crystallography as well as gas and liquid chromatography combined with mass spectrometry. Spectroscopic techniques have also been used, such as nuclear magnetic resonance, infrared and ultraviolet-visible spectroscopies. Results We presented the identification and the broad chemical characterization of etazene, a synthetic opioid that has recently been introduced on the illegal drug market. Conclusions In this paper, we described single-crystal X-ray, chromatographic and spectroscopic characterization of a synthetic opioid that emerged on the new psychoactive substance (NPS) market in Poland. To the best of our knowledge, this is the first full characterization of etazene. Analytical data presented in the work can be helpful in identification and detection of the NPS in forensic and clinical laboratories.


1992 ◽  
Vol 287 ◽  
Author(s):  
F. Babonneau ◽  
G. D. Soraru

ABSTRACTA commercial polycarbosilane was modified with various metallic alkoxides to get mixed ceramic precursors in the Si-M-C-O systems (M=Ti, Zr Al). Pyrolysis under ammonia leads to the formation of various ceramic materials depending on the nature of M : Si3N4/TiN, Si3N4/ZrO2 or β′-SiAlON phases.The polymer-to-ceramics conversion have been studied by MAS-NMR (29 Si, 27Al) and X-ray absorption (Ti K-edge). This paper will show how these two complementary spectroscopic techniques can be used to follow the nitridation process by probing local environments of different elements. In addition, it will be pointed out how X-ray absorption can be a powerful tool for the detection of the crystallization of nitride cubic phases.


2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
P. V. Oliveira ◽  
M. S. S. Viana ◽  
O. A. Barros ◽  
P. T. C. Freire ◽  
F. I. Bezerra ◽  
...  

The preservation of fossils depends on several interactions of organic and inorganic chemical processes. The hard parts, which are more suitable for fossilization, might record valuable information of biogenic processes, while the taphonomic characteristics supply information on postmortem chemical transformation. Here, X-ray fluorescence, X-ray diffraction, and infrared spectroscopy analyses were carried out in Early Eoholocene fragments of bones collected from the subsurface at Gruta do Urso Fóssil, Ubajara National Park, northeast of Ceará State in Brazil. It is suggested a lower degree of decomposition, a preservation of the original mineral composition, along with some incidence of encrustation, and the occurrence of different animal species are analyzed. These preliminary data serve as a basis for future studies involving fossil biota from the deposits of Gruta do Urso Fóssil using spectroscopic techniques.


2013 ◽  
Vol 2013 ◽  
pp. 1-10
Author(s):  
Gauri D. Bajju ◽  
Deepmala ◽  
Sunil Kumar Anand ◽  
Sujata Kundan ◽  
Narinder Singh

A series of aluminium(III)-p-methyl-meso-tetraphenylporphyrin (p-CH3TPP-Al(III)) containing axially coordinated salicylate anion [p-CH3TPP-Al-X)], where X = salicylate (SA), 4-chlorosalicylate (4-CSA), 5-chlorosalicylate (5-CSA), 5-flourosalicylate (5-FSA), 4-aminosalicylate (4-ASA), 5-aminosalicylate (5-ASA), 5-nitrosalicylate (5-NSA), and 5-sulfosalicylate (5-SSA), have been synthesized and characterized by various spectroscopic techniques including ultraviolet-visible (UV-vis), infrared (IR) spectroscopy, proton nuclear magnetic resonance (1H NMR) spectroscopy,13C NMR, and elemental analysis. A detailed study of electrochemistry of all the synthesized compounds has been done to compare their oxidation and reduction mechanisms and to explain the effect of axial coordination on their redox properties.


2011 ◽  
Vol 8 (s1) ◽  
pp. S113-S118
Author(s):  
Disha Jain Alok Chaturvedi ◽  
R.K. Upadhayay

The reaction of lead(II) dichloride with ammonium salts ofO,O'-ditolyldithiophosphoric acid have been carried out in 1:2 molar ratio by refluxing in benzene. These compounds have been further used to synthesize the adduct of the type lead(II)bis{O,O'-ditolyldithiophosphates}.2,2'-bipyridyl and lead(II)bis {O,O'-ditolyldithiophosphates}.1,10-phenanthroline by the reaction of lead(II)bis{O,O'-ditolyldithiophosphates} and 2,2'-bipyridyl and 1,10-phenanthro-line in the presence of unimolar dichloromethane and ethanol. All these complexes have been characterized by spectroscopic techniques such as IR,1H NMR and31P NMR. On the basis of spectroscopic studies tetracoordinated nature of lead atom in ditolyldithiophosphates complexes and hexacoordinated nature in their adducts have been established.


1990 ◽  
Vol 180 ◽  
Author(s):  
Florence Babonneau ◽  
Patrice Barre ◽  
Jacques Livage ◽  
Michel Verdaguer

ABSTRACTPolytitanocarbosilane precursor for SiC/TiC ceramics was characterized by various spectroscopic techniques (29Si and 13C CP MAS NMR, Ti K-edge XANES and EXAFS) in order to follow how titanium ions are incorporated into the polycarbosilane-based polymer. This polymer has been fired in argon atmosphere, and the evolution of the local environments of Si and Ti atoms, during the pyrolysis process, have been followed using 29Si MAS-NMR and Ti K-edge X-ray absorption: this study reveals the formation of Si-O bonds above 500°C, while Ti-C bonds clearly appear around 800°C. Above 1000°C, Si-O bonds are consumed by reaction with excess carbon and the system finally crystallizes into SiC/TiC mixture above 1200°C.


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