scholarly journals SYNTHESIS OF MACROCYCLES FROM COMPLEX NICKEL SALTS

Author(s):  
Д.С. Ильясов ◽  
С.Г. Ильясов

Исследовано взаимодействие комплексной соли хлорида никеля (II) с диаминомочевиной в присутствии глиоксаля. Получены различные комплексные соли катионного типа на основе никеля (II) с диаминомочевиной и на их основе были синтезированы соответствующие макроциклические соединения. Полученные комплексы и макроциклы исследованы физико-химическими методами анализа. The interaction of a complex salt of nickel (II) chloride with diamino urea in the presence of glyoxal was studied. Various complex salts of the cationic type based on nickel (II) with diamino urea were obtained and the corresponding macrocyclic compounds were synthesized on their basis. The resulting complexes and macrocycles were studied by physicochemical methods of analysis.

The intense red colour and the stability of the product of reaction between ferrous salts and αα′ dipyridyl has remained a striking instance of complex salt formation since the discovery of this dipyridyl by Blau (1888). Although for obvious reasons this compound would seem a good reagent for the colorimetric estimation of iron, it has never been used to any extent for the purpose, without doubt because there are other more sensitive and accessible reagents. It seems, however, to possess unique advantages for the study of iron in connection with living material, and on its account it was thought advisable to bring αα′ dipyridyl, as a reagent for iron, to the notice of biologists. αα′ dipyridyl was first prepared by Blau (1888) by distilling the copper salt of α picolinic acid; the yield is small, but this method has the advantage of readily yielding a pure product. Recently Hein and Retter (1928) have found a relatively simple method of preparation by heating pyridine in a sealed tube with an oxidising agent such as ferric chloride, which removes hydrogen without the formation of water. This method though more economical needs greater manipulation to produce the substance in a state of purity. Smith (1926) isolated the same substance by the oxidation of sodium pyridines with dry air above 100° C. The ferrous complex salts were examined by Werner (1912) who showed that they could be resolved into two optical isomers. The ferrous salts of αα′ dipyridyl have the formula [Fe(C 10 H 8 N 3 ) 3 ]X 2 (Blau, 1898) where X is a monovalent acid radicle, and from the fact that the optical isomers do not racemize at once (Werner, 1912) dissociation into free ferrous salts must be relatively slight. They differ from the normal ferrous salts in not being eaily oxidised, in fact only powerful agents such as permanganate or chlorine oxidise them to a blue compound. This latter compound, which should be the ferric complex salt, is not obtained directly from ferric salts and αα′ dipyridyl and passes very easily into the red ferrous salt.


1982 ◽  
Vol 95 (1) ◽  
pp. 95-103 ◽  
Author(s):  
P. L. Storring ◽  
P. H. Corran ◽  
Rose E. Gaines Das ◽  
D. H. Calam

The preparation and nature of the International Reference Preparation of Gonadorelin for Bioassay (IRP; coded 77/596) are described. The IRP was studied by four laboratories in four countries and compared, using physicochemical methods of analysis, various bioassay procedures and immunoassay, with preparations of synthetic luteinizing hormone releasing hormone (LH-RH) produced by different manufacturers. Analyses by thin-layer chromatography and by reverse-phase high-performance liquid chromatography (HPLC) indicated some heterogeneity of the peptide present in most of these preparations of synthetic LH-RH, including that of the IRP; the latter preparation appeared to be 88·3% (w/w) pure, judged by HPLC. The data from the collaborative study suggested that each ampoule of the IRP contains approximately 31 nmol LH-RH. The IRP appeared to be suitable to serve as an international reference preparation for bioassay since its behaviour was similar in different bioassays, so far as this could be examined, to that of the other preparations of LH-RH with which it was compared. Furthermore, the biological activities of different preparations of LH-RH, assessed in terms of the IRP, appeared to correlate with their degrees of purity assessed by physicochemical methods, suggesting that the peptides other than LH-RH present in the IRP did not contribute significantly to the biological activity of the preparation in these assay procedures. The limited data available suggested that the IRP might also be suitable as a reference preparation for immunoassay. The ampouled preparation, coded 77/596, was therefore established by the World Health Organization as the International Reference Preparation of Gonadorelin for Bioassay and assigned a unitage of 31 i.u./ampoule on the basis that the i.u. is represented by 1 nmole of LH-RH.


2021 ◽  
Vol 13 (1) ◽  
pp. 105-108
Author(s):  
Denis Yu. Kornilov ◽  
◽  
◽  

The material of the defense of the dissertation for the degree of Doctor of Technical Sciences is presented - the first doctoral dissertation in Russia on graphene topics. The relevance of the search for new electroactive nanomaterials for current sources of portable electronic equipment in conditions of its high energy consumption with its miniaturization and increase in performance is noted, the object of research is characterized - graphene oxide as a cathode material for lithium chemical current sources, the formulation of research tasks is formulated, the physicochemical methods of analysis.


2021 ◽  
Vol 10 (1) ◽  
pp. 83-89
Author(s):  
V. G. Luzhanin ◽  
A. K. Whaley ◽  
A. O. Ponkratova ◽  
E. A. Grishukova ◽  
I. S. Suloev ◽  
...  

Introduction. Among the different groups of drugs, diuretics are one the most popular classes that have been used for treatment of cardiovascular system and kidney diseases. At the same time, synthetic diuretics which are widely used, cause large amounts of side effects, such as violation of electrolyte, acid-base and water balances, carbohydrate and lipid metabolism. Therefore, it is important to search for individual compounds of plant origin – potential pharmaceutical substances for the treatment of urinary tract diseases. In this study individual compounds were isolated from the terrestrial parts of Ononis arvensis L. and Solidago canadensis L. The diuretic activity of the summary extracts of Ononis arvensis and Solidago canadensis has previously been proven.Aim. Method development for the isolation of individual compounds, using modern physicochemical methods of analysis, from the terrestrial parts of Ononis arvensis and Solidago canadensis and the elucidation of their structure.Materials and methods. Aerial parts of Ononis arvensis and Solidago canadensis were collected in the Saint Petersburg State Chemical-Pharmaceutical University (SPCPU) Nursery Garden of Medicinal Plants (Leningrad region, Vsevolozhsky district, Priozersk highway, 38 km) in August 2019 and identified by Dr. Goncharov Mikhail of the Saint-Petersburg chemical-pharmaceutical university, Saint-Petersburg, Russia. Fraction analysis were preformed with analytical high-performance liquid chromatography using a LC-20 Prominence (Shimadzu corp., Japan) with a SPD-M20A diode-array detector. Isolation of individual compounds was carried out by preparative high-performance liquid chromatography using a Smartline (Knauer, Germany). The structures of the isolated compounds were elucidated using 1D and 2D NMR experiments (Bruker Avance III 400 MHz) along with HR-ESI-MS (Bruker Micromass Q-TOF).Results and discussion. Using the developed methods, from the aerial part of the field restharrow (O. arvensis) we managed to isolate and characterised three individual compounds (1-3). Compounds 1 and 2 are isloflavonoids – pseudobaptigenin-7-О-ß-D-glucopyranoside and formononetin-7-О-ß-D-glucopyranoside, respectively. Compound (3) is a flavonoid – kaempferol-3-O-ß-D-glucopyranoside (astragalin). All compounds were isolated for O. arvansis for the first time. Along with this, four individual compounds (4-7) were isolated from the aerial part of the canadian goldenrod (S. canadensis), namely, quercetin-3-O-ß-D-6''-acetylglucopyranoside, isoramnetin-3-О-ß-D-rutinoside (narcissin), quercetin-3-О-rutinoside (rutin) and quercetin, respectively.Conclusion. As a result of the research, methods have been developed for the isolation of 7 individual compounds, using modern physicochemical methods of analysis, from the aerial parts of Ononis arvensis and Solidago canadensis, the structures of all the isolated compounds were elucidated. Future assessment of the isolated compounds biological activity is presumed.


1971 ◽  
Vol 5 (12) ◽  
pp. 759-760
Author(s):  
S. L. Belen'kaya ◽  
G. P. Tikhomirova ◽  
L. A. Prokhorenko

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