scholarly journals New development of laser-based techniques in applications of thin-layer chromatography, microprobe elemental analysis and gas phase pyrolysis

1990 ◽  
Author(s):  
Jianzhong Zhu
Author(s):  
J.V. Guna ◽  
V.N. Bhadani ◽  
H.D. Purohit ◽  
Dipak M. Purohit

2- Methoxy – 6 - {4' - [(4'''- Chlorophenyl) (phenyl) methyl amino] phenyl} - 4 - aryl nicotinonitrile (3a-3l) and 2-Amino-6-{4'-[(4'''-Chlorophenyl)(phenyl)methyl amino]phenyl}-4-aryl nicotinonitrile (4a-4l) have been synthesized. The products have been assayed for their antimicrobial activity against Gram +ve, Gram -ve bacteria and fungi. The structure of the products has been elucidated by IR, 1H-NMR, mass spectral data, elemental analysis and thin layer chromatography.


1980 ◽  
Vol 58 (7) ◽  
pp. 723-726 ◽  
Author(s):  
Patricia F. Currie ◽  
J. Wilson Quail ◽  
John A. Weil

The reaction between 2,2-diphenyl-1-picrylhydrazyl and bromine in solution bas been studied at several temperatures. Despite the literature, reporting simple phenyl bromination products, a substantial yield of nitration products is observed. These have been identified by use of thin-layer chromatography, mass spectrometry, nuclear magnetic resonance, and elemental analysis. Among various products, 2-(p-nitrophenyl)-2-phenyl-1-picrylhydrazine is a major one at room temperature and above. It is thought that this compound is formed by reaction of DPPH with NO2, displaced from ortho nitro groups in the picryl rings by bromine. Yields were found to vary, depending on experimental conditions, with the temperature and the rate of bromine addition as primary controlling factors.


Author(s):  
D. V. Dovbnia ◽  
A. H. Kaplaushenko ◽  
Yu. S. Frolova

The aim of the work is to develop preparative methods for the synthesis of 2-((5-(2,4- and 3,4-dimethoxyphenyl)-3H-1,2,4-triazole-3-yl)thio)acetic acids, to study the esterification reaction in this regard, to study physical and chemical properties of the obtained substances, and to predict their toxicity. Materials and methods. Compounds were synthesized using reagents and solvents qualified as “ch.p.”. The IUPAC nomenclature as supplemented was used during the preparation. The melting temperature was determined with the capillary method according to HFC (2.2.14) on the device PTP (M). Elemental analysis was determined with the ELEMENTAR vario EL cube analyzer (manufactured in Germany) (standard – sulfonamide). IR spectra were recorded using spectrophotometer Specord M-80 (manufactured in Germany) within the range of 4000–500 cm-1 (scanning was performed under the following conditions: slot program 3.0, time constant – τ = 3 s, scanning time 34 min, samples were analyzed in the form of tablets with potassium bromide). 1H NMR spectra were recorded using Varian VXR-300 spectrophotometer (manufactured in the USA), dimethyl sulfoxide-D6 solvent, and tetramethylsilane was used as an internal standard. The spectra were decoded using the computer program ADVASP 1.43. Thin layer chromatography was performed using Sorbfil plates (analytical, size 10 × 15 cm, base: polymer substrate, sorbent: silica gel STX-1A, grain: 5–17 μm, layer thickness: 110 m combination – silicazole). Results. The synthesis of new 2-((5-(2,4- and 3,4-dimethoxyphenyl)-3H-1,2,4-triazole-3-yl)thio)acetic acids was carried out. These products became a basis for synthesis of a number of relevant esters. Physical and chemical properties were investigated for the synthesized compounds. The structure of the obtained substances was confirmed by elemental analysis, IR-spectroscopy, 1H NMR-spectrometry, and their individuality were established by thin-layer chromatography. Computer GUSAR-online prediction of acute toxicity of 2-((5-(2,4- and 3,4-dimethoxyphenyl)-3H-1,2,4-triazole-3-yl)thio)acetic acids and their esters was performed. Conclusions. Preparative methods for the synthesis of 2-((5-(2,4- and 3,4-dimethoxyphenyl)-3H-1,2,4-triazole-3-yl)thio)acetic acids have been developed, for which esterification reactions have been studied. Thus, physical and chemical properties of the received substances were investigated, and indicators of their toxicity were predicted.


2020 ◽  
Vol 62 (6) ◽  
pp. 40-43
Author(s):  
Elena V. Kuvaeva ◽  
◽  
Denis A. Kolesnik ◽  
Ksenia E. Kirpikova ◽  
Igor P. Yakovlev ◽  
...  

In this paper, 6-hydroxypyrimidine-4 (3Н)-one derivatives are considered as promising syntones for the creation of new biologically active substances. This is useful since the pyrimidine fragment is a structural component of nucleic acid bases (cytosine, thymine, uracil), uric and orotic acids, coenzymes (flavins and xanthins), a number of vitamins (folic acid, thiamine, pyridoxine, riboflavin). It is worth noting that the pharmaceutical market is widely represented with antitumor (methotrexate, imatinib, tegafur); antiviral (stavudine, zalcitabine, lamivudine, zidovudine, acyclovir, idoxuridine); immunostimulatory (isophone) and sedative drugs (phenobarbital, sodium ethaminal) based on compounds including the pyrimidine cycle. The purpose of the present work is to develop a method for producing new 2,3-diphenyl-5-(alkyl/ phenyl)-6-hydroxypyrimidin-4(3Н)-ones, proving their structure and individuality by NMR spectroscopy and mass spectrometry, elemental analysis and thin-layer chromatography. As a method of producing new 6-hydroxypyrimidin-4(3Н)-ones, a method of condensing N-phenyl-benzenecarboxymidamide with 2-substituted propanedioyldichlorides in the medium of an aprotic non-polar solvent – o-xylene is proposed. The desired products are isolated from the reaction mass using solvent distillation and a reprecipitation method. It was found that maximum yields are achieved with constant stirring of a suspension of N-phenylbenzenecarboxymidamide with a solution of 2-substituted propanedioyl dichloride in o-xylene and further heating of the reaction mass at 144 °C for 4 hours. The individuality of the synthesized compounds was confirmed by thin layer chromatography on Sorbfil® plates in the methanol-dichloroethane (1:9) system, and their structure was proved using modern physicochemical analysis methods: proton magnetic resonance spectroscopy, NMR С13 spectroscopy, mass spectroscopy and elemental analysis.


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