Pub Date : 2019-10-31DOI: 10.37952/roi-jbc-01/19-60-10-88
L. Maskaeva, V. M. Yurk, Anastasia V. Belceva, I. V. Zarubin, A. D. Kutyavina, V. F. Markov
Calculation of ionic equilibria in the reaction system for synthesis of PbSe thin films was carried out. Three reaction systems containing the following combinations of reagents were considered: sodium citrate with liquid ammonia and sodium selenosulfate (system 1) or selenourea (system 2) used as chalcogenizer, ethilendiamine, sodium acetate and selenourea (system 3).The main lead complex compoundsprevented the fast PbSe formation in system 1 and 2 in region of pH of intensive selenosulfate and selenourea decomposition were hydroxo-citrate complexes. In the system 3 complexes with ethilendiamine and acetate-ions played the most significant role. For evaluating the deposition conditions of the main and impurity phases (metal hydroxides and cyanamides) by thermodynamic calculations taking into account the sizes of critical nucleis, the boundary conditions and regions of formation of PbSe, Pb(OH)2, PbCN2 in the studied reaction systems were found. The calculation results are presented in the form of three-dimensional dependencies in the coordinates “indicator of the initial concentration of the metal salt – pH of the solution – ligand concentration” and “indicator of the initial concentration of the metal salt – pH of the solution – concentration of the chalcogenizer”. Based on the calculations and preliminary experiments, the compositions of the discussed reaction mixtures were formed for the chemical bath deposition of PbSe films, which, in addition to the main components, included a dopant in the form of ammonium iodide. In the synthesis process at a temperature of 353 K (system 1 and 2) for 60 minutes and 308 K for 90 minutes (system 3), using all the studied reaction systems on glass substrates, homogeneous PbSe layers with a thickness of ~500 to ~700 nm were obtained. The ratio between the main elements of Pb and Se in the film varies between 0.98-1.32, and the iodine content is 7-11 at.% depending on the composition of the reaction bath.
{"title":"Chemical bath synthesis of metal chalcogenide films. Part 42. Experimental verification of the deposition regions of PbSe by sodium selenosulfate and selenourea in the presence of various ligands","authors":"L. Maskaeva, V. M. Yurk, Anastasia V. Belceva, I. V. Zarubin, A. D. Kutyavina, V. F. Markov","doi":"10.37952/roi-jbc-01/19-60-10-88","DOIUrl":"https://doi.org/10.37952/roi-jbc-01/19-60-10-88","url":null,"abstract":"Calculation of ionic equilibria in the reaction system for synthesis of PbSe thin films was carried out. Three reaction systems containing the following combinations of reagents were considered: sodium citrate with liquid ammonia and sodium selenosulfate (system 1) or selenourea (system 2) used as chalcogenizer, ethilendiamine, sodium acetate and selenourea (system 3).The main lead complex compoundsprevented the fast PbSe formation in system 1 and 2 in region of pH of intensive selenosulfate and selenourea decomposition were hydroxo-citrate complexes. In the system 3 complexes with ethilendiamine and acetate-ions played the most significant role. For evaluating the deposition conditions of the main and impurity phases (metal hydroxides and cyanamides) by thermodynamic calculations taking into account the sizes of critical nucleis, the boundary conditions and regions of formation of PbSe, Pb(OH)2, PbCN2 in the studied reaction systems were found. The calculation results are presented in the form of three-dimensional dependencies in the coordinates “indicator of the initial concentration of the metal salt – pH of the solution – ligand concentration” and “indicator of the initial concentration of the metal salt – pH of the solution – concentration of the chalcogenizer”. Based on the calculations and preliminary experiments, the compositions of the discussed reaction mixtures were formed for the chemical bath deposition of PbSe films, which, in addition to the main components, included a dopant in the form of ammonium iodide. In the synthesis process at a temperature of 353 K (system 1 and 2) for 60 minutes and 308 K for 90 minutes (system 3), using all the studied reaction systems on glass substrates, homogeneous PbSe layers with a thickness of ~500 to ~700 nm were obtained. The ratio between the main elements of Pb and Se in the film varies between 0.98-1.32, and the iodine content is 7-11 at.% depending on the composition of the reaction bath.","PeriodicalId":9405,"journal":{"name":"Butlerov Communications","volume":"33 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-10-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91345995","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2019-10-31DOI: 10.37952/roi-jbc-01/19-60-10-110
R. Kolmykov, Аnna V. Petrushina, S. Sozinov
This work is devoted to determining the chemical composition of coal ashes. We used the optical emission spectrometry with inductively coupled plasma and laser sampling as a research method. The aim of the work is to determine the limits of detection (LoDs) and quantitative determination (LoQs) of elements in ashes using polyvinyl alcohol (PVA) and microcrystalline cellulose (MCC) as binders. In this work, analytical signals of Al, Ba, Be, Ca, Cr, Cu, Fe, K, La, Li, Mg, Mn, Na, Ni, P, Pb, S, Sc, Sr, Ti, Y, V, Zr, and Zn were analyzed in tablets obtained from the standard samples ZUK-1, ZUK-2, SG-1A, SG-3, SGD-2A, and SO-1, compacted using PVA and MCC, as well as from binding agents themselves. To obtain compact materials based on fly ash and geological materials, both binders are suitable if their chemical purity is enough for analysis. However, when using both MCC and PVA, some drawbacks were identified. The intensities of analytical lines of the elements were determined lower during the ablation of compact ashes with MCC than with PVA. The signal-background ratio is lower when using MCC as a binder material compared with compacts based on PVA. However, the highest grade PVA according to GOST 10779-78, used in the work, contains an admixture of sodium, about 0.06 w. %, which interferes with quantitative measurements if the sodium content in the sample is comparable to this value, which can be extremely rare in the analysis of fly ashes.
这项工作致力于测定煤灰的化学成分。我们采用电感耦合等离子体和激光采样的光学发射光谱法作为研究方法。以聚乙烯醇(PVA)和微晶纤维素(MCC)为粘结剂，确定灰中元素的检出限(LoDs)和定量测定(LoQs)。在这项工作中，分析了Al、Ba、Be、Ca、Cr、Cu、Fe、K、La、Li、Mg、Mn、Na、Ni、P、Pb、S、Sc、Sr、Ti、Y、V、Zr和Zn的分析信号，这些信号来自于标准样品ZUK-1、ZUK-2、SG-1A、SG-3、SGD-2A和SO-1，用PVA和MCC压实，以及结合剂本身。为了获得基于粉煤灰和地质材料的致密材料，如果它们的化学纯度足够分析，这两种粘合剂都是合适的。然而，当同时使用MCC和PVA时，发现了一些缺点。用MCC烧蚀致密灰渣时测定的元素分析谱线强度低于用PVA烧蚀时测定的。与PVA基压实材料相比，MCC基压实材料的信本比更低。然而，根据GOST 10779-78，在工作中使用的最高等级的PVA含有钠的混合物，约0.06 w. %，如果样品中的钠含量与此值相当，则会干扰定量测量，这在分析粉煤灰时是极其罕见的。
{"title":"Influence of the binder used in pressing ash for laser sampling on the quality of analytical signals of the elements detected","authors":"R. Kolmykov, Аnna V. Petrushina, S. Sozinov","doi":"10.37952/roi-jbc-01/19-60-10-110","DOIUrl":"https://doi.org/10.37952/roi-jbc-01/19-60-10-110","url":null,"abstract":"This work is devoted to determining the chemical composition of coal ashes. We used the optical emission spectrometry with inductively coupled plasma and laser sampling as a research method. The aim of the work is to determine the limits of detection (LoDs) and quantitative determination (LoQs) of elements in ashes using polyvinyl alcohol (PVA) and microcrystalline cellulose (MCC) as binders. In this work, analytical signals of Al, Ba, Be, Ca, Cr, Cu, Fe, K, La, Li, Mg, Mn, Na, Ni, P, Pb, S, Sc, Sr, Ti, Y, V, Zr, and Zn were analyzed in tablets obtained from the standard samples ZUK-1, ZUK-2, SG-1A, SG-3, SGD-2A, and SO-1, compacted using PVA and MCC, as well as from binding agents themselves. To obtain compact materials based on fly ash and geological materials, both binders are suitable if their chemical purity is enough for analysis. However, when using both MCC and PVA, some drawbacks were identified. The intensities of analytical lines of the elements were determined lower during the ablation of compact ashes with MCC than with PVA. The signal-background ratio is lower when using MCC as a binder material compared with compacts based on PVA. However, the highest grade PVA according to GOST 10779-78, used in the work, contains an admixture of sodium, about 0.06 w. %, which interferes with quantitative measurements if the sodium content in the sample is comparable to this value, which can be extremely rare in the analysis of fly ashes.","PeriodicalId":9405,"journal":{"name":"Butlerov Communications","volume":"38 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-10-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80092565","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2019-10-31DOI: 10.37952/roi-jbc-01/19-60-10-124
A. V. Burchakov, I. Garkushin, S. N. Milov, M. A. Sukharenko
The paper presents the results of a theoretical study of the phase complex of a three-component system consisting of tungstates, molybdates and sodium chlorides for equilibrium "liquid - solid". Previously, a literature review was conducted on data on phase equilibria in the condensed state of individual salts, binary faceting systems. In two NaCl-Na2MoO4 and NaCl-Na2WO4 binary systems, a eutetic equilibrium is observed with the formation of solid phases corresponding to the system components and Na3ClMoO4 and Na3ClWO4, and in binary faceting system Na2MoO4 – Na2WO4, one phase of a continuous series of solid solutions crystallizes. Based on the mathematical model of the molar balance, one can uniquely determine the quantities of reaction products, the molecular formulas of solid solutions, and the equations of chemical reactions for an arbitrary mixture of system components. This model represents a set of algebraic equations by which the balance is calculated. To build a 3D computer model, the paper presents the equations for the conversion of coordinates from barycentric to Cartesian. The model is implemented in concentration-temperature coordinates using the KOMPAS-3D program using experimental data on the system. With 3D model it is possible to conduct a preliminary a priori forecast of phase equilibria in order to identify the structure of phase diagrams at the qualitative and quantitative levels. The projection of the crystallization polytherm onto the square of the compositions is represented by three fields of solid solutions – NaCl, Na3ClMoxW1-xO4 and Na2MoxW1-xO4. Isothermal and polythermal sections were constructed. The system implements di- and monovariant equilibria. A diagram of the material balance of crystallizing phases is constructed. The paper presents the calculation of the ratio of equilibrium phases, as well as their qualitative and quantitative composition for the two-phase and three-phase regions according to the coordinates of the points - the vertices of the conode segments and conode triangles, which are extracted from the 3D model. The calculation is implemented for a given composition and temperature.
{"title":"Forecasting of phase equilibria in the system NaCl-Na2MoO4-Na2WO4 at the liquid-solid interface","authors":"A. V. Burchakov, I. Garkushin, S. N. Milov, M. A. Sukharenko","doi":"10.37952/roi-jbc-01/19-60-10-124","DOIUrl":"https://doi.org/10.37952/roi-jbc-01/19-60-10-124","url":null,"abstract":"The paper presents the results of a theoretical study of the phase complex of a three-component system consisting of tungstates, molybdates and sodium chlorides for equilibrium \"liquid - solid\". Previously, a literature review was conducted on data on phase equilibria in the condensed state of individual salts, binary faceting systems. In two NaCl-Na2MoO4 and NaCl-Na2WO4 binary systems, a eutetic equilibrium is observed with the formation of solid phases corresponding to the system components and Na3ClMoO4 and Na3ClWO4, and in binary faceting system Na2MoO4 – Na2WO4, one phase of a continuous series of solid solutions crystallizes. Based on the mathematical model of the molar balance, one can uniquely determine the quantities of reaction products, the molecular formulas of solid solutions, and the equations of chemical reactions for an arbitrary mixture of system components. This model represents a set of algebraic equations by which the balance is calculated. To build a 3D computer model, the paper presents the equations for the conversion of coordinates from barycentric to Cartesian. The model is implemented in concentration-temperature coordinates using the KOMPAS-3D program using experimental data on the system. With 3D model it is possible to conduct a preliminary a priori forecast of phase equilibria in order to identify the structure of phase diagrams at the qualitative and quantitative levels. The projection of the crystallization polytherm onto the square of the compositions is represented by three fields of solid solutions – NaCl, Na3ClMoxW1-xO4 and Na2MoxW1-xO4. Isothermal and polythermal sections were constructed. The system implements di- and monovariant equilibria. A diagram of the material balance of crystallizing phases is constructed. The paper presents the calculation of the ratio of equilibrium phases, as well as their qualitative and quantitative composition for the two-phase and three-phase regions according to the coordinates of the points - the vertices of the conode segments and conode triangles, which are extracted from the 3D model. The calculation is implemented for a given composition and temperature.","PeriodicalId":9405,"journal":{"name":"Butlerov Communications","volume":"100 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-10-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77050163","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2019-10-31DOI: 10.37952/roi-jbc-01/19-60-10-48
E. Gorshkova, T. V. Vdovina
A comparative assessment of the currently used methods for determining the resistance of materials to the penetration of microbial suspensions is carried out. The essence of the analyzed methods consists in comparing the number of colonies of microorganisms grown through the test sample with the number of colonies of microorganisms grown on control samples. To standardize the materials, the method GOST standard 12.4.136-84 of 04/01/1990, of 01/04/1990 “Occupational safety standards system. Personal protective equipment, a method for determining the permeability of microorganisms ", establish a protection class; method ISO 22610: 2006 (R) “Surgical sheets, gowns and suits for clean rooms for patients, medical personnel and equipment used as medical devices, test method for determining the resistance to penetration of wet bacterial environments” determines the total penetration coefficient indicated in addition to the usual labeling of medical materials, and may be the interest for products to enter the international market. The methods described by researchers Ransjo U., Hambraeus A., Blom A.W., Estela C.M., Bowker K.E., MacGowan A.P., Hardy J., take place in laboratory tests for comparative studies. As a test culture was used Bacillus subtilis. Nonwovens were analyzed: three-layer Medicase RKV, Belgium and Softess Dupon, USA. The results of assessing the permeability of materials by the microbial suspension of Bacillus subtilis, obtained by various methods, correlate with each other. Medicase RKV was found to have poor barrier properties and is not resistant to microbial entry. The material Softess Dupon has good barrier properties and is relatively resistant to the penetration of microorganisms: it has a 5th grade of protection, a bacterial threat of T – 60, a coefficient of penetration through the barrier of Cvp – 0.75, a bacterial index lv – 5.67, characterized by meager growth of microorganisms upon contact of the material with bacteria for 15, 30, 60 minutes and excessive growth – upon contact for 90 minutes.
{"title":"Comparative evaluation of methods for determining the resistance of materials to penetration of microbial suspensions","authors":"E. Gorshkova, T. V. Vdovina","doi":"10.37952/roi-jbc-01/19-60-10-48","DOIUrl":"https://doi.org/10.37952/roi-jbc-01/19-60-10-48","url":null,"abstract":"A comparative assessment of the currently used methods for determining the resistance of materials to the penetration of microbial suspensions is carried out. The essence of the analyzed methods consists in comparing the number of colonies of microorganisms grown through the test sample with the number of colonies of microorganisms grown on control samples. To standardize the materials, the method GOST standard 12.4.136-84 of 04/01/1990, of 01/04/1990 “Occupational safety standards system. Personal protective equipment, a method for determining the permeability of microorganisms \", establish a protection class; method ISO 22610: 2006 (R) “Surgical sheets, gowns and suits for clean rooms for patients, medical personnel and equipment used as medical devices, test method for determining the resistance to penetration of wet bacterial environments” determines the total penetration coefficient indicated in addition to the usual labeling of medical materials, and may be the interest for products to enter the international market. The methods described by researchers Ransjo U., Hambraeus A., Blom A.W., Estela C.M., Bowker K.E., MacGowan A.P., Hardy J., take place in laboratory tests for comparative studies. As a test culture was used Bacillus subtilis. Nonwovens were analyzed: three-layer Medicase RKV, Belgium and Softess Dupon, USA. The results of assessing the permeability of materials by the microbial suspension of Bacillus subtilis, obtained by various methods, correlate with each other. Medicase RKV was found to have poor barrier properties and is not resistant to microbial entry. The material Softess Dupon has good barrier properties and is relatively resistant to the penetration of microorganisms: it has a 5th grade of protection, a bacterial threat of T – 60, a coefficient of penetration through the barrier of Cvp – 0.75, a bacterial index lv – 5.67, characterized by meager growth of microorganisms upon contact of the material with bacteria for 15, 30, 60 minutes and excessive growth – upon contact for 90 minutes.","PeriodicalId":9405,"journal":{"name":"Butlerov Communications","volume":"14 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-10-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73946472","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2019-10-31DOI: 10.37952/roi-jbc-01/19-60-10-60
E. V. Ferubko, V. N. Zelenkov, Tamara D. Dergaeva, A. Lapin
At present, the expansion of research to find sources for obtaining new effective and safe medicines of plant origin, including those used in gastroenterological practice, is a pressing task of medical science, considering that the range of medicinal plant drugs used in practical health care is more than 40%. The article presents the results of biochemical study of total antioxidant activity of anti-ulcer collection of plant origin and its individual components. We show that it consists of the leaves of the planter large (Plantago major L.), grass of a sushchenitsa uliginose (Gnaphalium uliginosum L.), rhizomes and roots of the devisil high (Inula helenium L.), flowers of the chamomile pharmacy (Matricaria chamomilla L.), the roots of licorice naked (Glycyrrhiza glabra L.), grass of bird's mountain (Polygonum aviculare L.), leaves of the nettle (Urtica dioica L.), fruits of a mountain ash ordinary (Sorbus aucuparia L.) and its individual components have pronounced antioxidant activity. The greatest activity was found in the roots of licorice naked, grass of bird 's mountain and flowers of chamomile pharmacy. Total antioxidant activity of water extraction of collection recovery at 6.34% from exceeded the calculated value obtained by summing the activities of the individual components of the collection, which indicates the presence of synergy in their action, which may be of importance for use in the treatment and prevention of diseases in gastroenterological practice. The detected increase in the antioxidant activity of the new collection compared to the effects of its individual components allows it to be considered as a promising dosage form for the treatment and prevention of gastroenterological diseases.
{"title":"The study of the antioxidant activity of the antiulcerous plant composition and its components","authors":"E. V. Ferubko, V. N. Zelenkov, Tamara D. Dergaeva, A. Lapin","doi":"10.37952/roi-jbc-01/19-60-10-60","DOIUrl":"https://doi.org/10.37952/roi-jbc-01/19-60-10-60","url":null,"abstract":"At present, the expansion of research to find sources for obtaining new effective and safe medicines of plant origin, including those used in gastroenterological practice, is a pressing task of medical science, considering that the range of medicinal plant drugs used in practical health care is more than 40%. The article presents the results of biochemical study of total antioxidant activity of anti-ulcer collection of plant origin and its individual components. We show that it consists of the leaves of the planter large (Plantago major L.), grass of a sushchenitsa uliginose (Gnaphalium uliginosum L.), rhizomes and roots of the devisil high (Inula helenium L.), flowers of the chamomile pharmacy (Matricaria chamomilla L.), the roots of licorice naked (Glycyrrhiza glabra L.), grass of bird's mountain (Polygonum aviculare L.), leaves of the nettle (Urtica dioica L.), fruits of a mountain ash ordinary (Sorbus aucuparia L.) and its individual components have pronounced antioxidant activity. The greatest activity was found in the roots of licorice naked, grass of bird 's mountain and flowers of chamomile pharmacy. Total antioxidant activity of water extraction of collection recovery at 6.34% from exceeded the calculated value obtained by summing the activities of the individual components of the collection, which indicates the presence of synergy in their action, which may be of importance for use in the treatment and prevention of diseases in gastroenterological practice. The detected increase in the antioxidant activity of the new collection compared to the effects of its individual components allows it to be considered as a promising dosage form for the treatment and prevention of gastroenterological diseases.","PeriodicalId":9405,"journal":{"name":"Butlerov Communications","volume":"33 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-10-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84659527","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2019-10-31DOI: 10.37952/roi-jbc-01/19-60-10-24
N. Lyukshenko, R. Nikitin, Y. Morozhenko
At present, benzodiazepine derivatives being used widely, they continue to occupy a leading position among the drugs of the anxiolytic group. Most anxiolytics of the benzodiazepine structure are derivatives of 1,4-benzodiazepine. The basis of the chemical benzodiazepine structure consists of a benzene ring connected to a seven-membered heterocyclic ring containing two nitrogen atoms (diazepine) at positions 1 and 4. All the benzodiazepine derivatives used in the clinic also have a second benzene ring attached to carbon. The presence of a halogen or a nitro group is essential to display its activity. Diazepam (1-methyl-5-phenyl-7-chloro-1,3-dihydro-2H- [1,4] benzodiazepin-2-one) is in the list of necessary and important medicinal products. The urgent issue is the development of a new method to synthesize 1-methyl-5-phenyl-7-chloro-1,3-dihydro-2H-[1,4]-benzodiazepines-2-one that would allow producing the drug in the required quantities and for mass consumption. The search for possible effective ways of synthesizing 1-methyl-5-phenyl-7-chlorine-1,3-dihydro-2H-[1,4]-benzodiazepines-2-one for manufacturing application is of great scientific and practical interest. The purpose of our work is to search for a rational method to synthesize the target product, experimental study of the chemical processes to develop the most optimal methods to produce the product. The technology to produce 1-methyl-5-phenyl-7-chlor-1,3-dihydro-2H-[1,4]-benzodiazepine-2-one on an industrial scale was developed. The synthesis of 2-benzoyl-2',4-dichloro-N-methylacetanilide by condensation of 2-methylamine-5-chlorobenzophenone with chloracetyl chloride in carbon tetrachloride without further treatment of the reaction mass with water and sodium carbonate was developed. The highest yield of 1-methyl-5-phenyl-7-chlorine-1,3-dihydro-2H-[1,4]-benzodiazepines-2-one was shown to be obtained if the cyclization reaction is carried out in isopropyl alcohol. The reaction mixture composition in interaction of 2-benzoyl- 2',4 -dichloro-N-methylacetanilide with urotropin plays the defining role in the formation of the target product.
{"title":"New technology to obtain 1-methyl-5-pnenyl-7-chloro- 1,3-dihydro-2H-[1,4]-benzodiazepine-2-one","authors":"N. Lyukshenko, R. Nikitin, Y. Morozhenko","doi":"10.37952/roi-jbc-01/19-60-10-24","DOIUrl":"https://doi.org/10.37952/roi-jbc-01/19-60-10-24","url":null,"abstract":"At present, benzodiazepine derivatives being used widely, they continue to occupy a leading position among the drugs of the anxiolytic group. Most anxiolytics of the benzodiazepine structure are derivatives of 1,4-benzodiazepine. The basis of the chemical benzodiazepine structure consists of a benzene ring connected to a seven-membered heterocyclic ring containing two nitrogen atoms (diazepine) at positions 1 and 4. All the benzodiazepine derivatives used in the clinic also have a second benzene ring attached to carbon. The presence of a halogen or a nitro group is essential to display its activity. Diazepam (1-methyl-5-phenyl-7-chloro-1,3-dihydro-2H- [1,4] benzodiazepin-2-one) is in the list of necessary and important medicinal products. The urgent issue is the development of a new method to synthesize 1-methyl-5-phenyl-7-chloro-1,3-dihydro-2H-[1,4]-benzodiazepines-2-one that would allow producing the drug in the required quantities and for mass consumption. The search for possible effective ways of synthesizing 1-methyl-5-phenyl-7-chlorine-1,3-dihydro-2H-[1,4]-benzodiazepines-2-one for manufacturing application is of great scientific and practical interest. The purpose of our work is to search for a rational method to synthesize the target product, experimental study of the chemical processes to develop the most optimal methods to produce the product. The technology to produce 1-methyl-5-phenyl-7-chlor-1,3-dihydro-2H-[1,4]-benzodiazepine-2-one on an industrial scale was developed. The synthesis of 2-benzoyl-2',4-dichloro-N-methylacetanilide by condensation of 2-methylamine-5-chlorobenzophenone with chloracetyl chloride in carbon tetrachloride without further treatment of the reaction mass with water and sodium carbonate was developed. The highest yield of 1-methyl-5-phenyl-7-chlorine-1,3-dihydro-2H-[1,4]-benzodiazepines-2-one was shown to be obtained if the cyclization reaction is carried out in isopropyl alcohol. The reaction mixture composition in interaction of 2-benzoyl- 2',4 -dichloro-N-methylacetanilide with urotropin plays the defining role in the formation of the target product.","PeriodicalId":9405,"journal":{"name":"Butlerov Communications","volume":"76 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-10-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78912884","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2019-10-31DOI: 10.37952/roi-jbc-01/19-60-10-1
Ekaterina M. Feklicheva (Okul), V. Rybakov, E. V. Babaev, E. N. Ofitserov
Based on the synthesized starting 2,4-dimethyl-6-oxo-1,6-dihydropyridin-3-carboxamide crystallizing as a dihydrate, 9 derivatives of it including O- and N-phenacyl substituted products were obtained through original rearrangements and cyclizations. The corresponding oxazolopyridinium perchlorate was obtained from the latter preparation in the presence of acid, from which indolysin was obtained under the action of a nitrogenous base. The obtained molecular and crystal structures of all the compounds were studied by single crystal diffraction: 2,4-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxamide dihydrate, 6-hydroxy-2,4-dimethyl-3-carbamoyl-pyridinium chloride monohydrate, 2,4-dimethyl-6-methoxypyridine-3-carboxamide, 1-[2-(4-methylphenyl)-2-oxoethyl]-2,4-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxamide, 2,4-dimethyl-6-oxo-1-[2- (4-[chlorophenyl)-2-oxoethyl]-1,6-dihydropyridine-3-carboxamide, 2,4-dimethyl-6-[2-(4-methylphenyl)-2-oxo-ethoxy]pyridin-3-carbox-amide, 2,4-dimethyl-6-[2-(4-chlorophenyl)-2-oxoethoxy] pyridin-3-carb xamide, 6-carbamoyl-2-(4-chlorophenyl)-5,7-dimethyl[1,3]oxazolo[3,2-a]pyridin-4 perchlorate, 7-methyl-5-morpholin-4 -yl-2-(4-chlorophenyl) indolysin-8-carboxamide. A structural analysis of the by-products of 1,4-bis (4-methylphenyl) butane-1,4-dione and 1,4-bis(4-chlorophenyl) butane-1,4-dione was also carried out. The synthesis methods of each of them are given. A comparative analysis of bond lengths, valence and torsion angles in similar fragments of molecules is carried out. Hydrogen bonds were revealed in the structures and their influence on the strength of molecular packing in crystals was shown. All structures of the studied compounds, in addition to XRD, are characterized by 1H NMR spectra.
{"title":"Synthesis and X-ray diffraction of derivatives 2,4-dimethyl-6-oxo-1,6-dihydropyridin-3-carboxamide","authors":"Ekaterina M. Feklicheva (Okul), V. Rybakov, E. V. Babaev, E. N. Ofitserov","doi":"10.37952/roi-jbc-01/19-60-10-1","DOIUrl":"https://doi.org/10.37952/roi-jbc-01/19-60-10-1","url":null,"abstract":"Based on the synthesized starting 2,4-dimethyl-6-oxo-1,6-dihydropyridin-3-carboxamide crystallizing as a dihydrate, 9 derivatives of it including O- and N-phenacyl substituted products were obtained through original rearrangements and cyclizations. The corresponding oxazolopyridinium perchlorate was obtained from the latter preparation in the presence of acid, from which indolysin was obtained under the action of a nitrogenous base. The obtained molecular and crystal structures of all the compounds were studied by single crystal diffraction: 2,4-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxamide dihydrate, 6-hydroxy-2,4-dimethyl-3-carbamoyl-pyridinium chloride monohydrate, 2,4-dimethyl-6-methoxypyridine-3-carboxamide, 1-[2-(4-methylphenyl)-2-oxoethyl]-2,4-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxamide, 2,4-dimethyl-6-oxo-1-[2- (4-[chlorophenyl)-2-oxoethyl]-1,6-dihydropyridine-3-carboxamide, 2,4-dimethyl-6-[2-(4-methylphenyl)-2-oxo-ethoxy]pyridin-3-carbox-amide, 2,4-dimethyl-6-[2-(4-chlorophenyl)-2-oxoethoxy] pyridin-3-carb xamide, 6-carbamoyl-2-(4-chlorophenyl)-5,7-dimethyl[1,3]oxazolo[3,2-a]pyridin-4 perchlorate, 7-methyl-5-morpholin-4 -yl-2-(4-chlorophenyl) indolysin-8-carboxamide. A structural analysis of the by-products of 1,4-bis (4-methylphenyl) butane-1,4-dione and 1,4-bis(4-chlorophenyl) butane-1,4-dione was also carried out. The synthesis methods of each of them are given. A comparative analysis of bond lengths, valence and torsion angles in similar fragments of molecules is carried out. Hydrogen bonds were revealed in the structures and their influence on the strength of molecular packing in crystals was shown. All structures of the studied compounds, in addition to XRD, are characterized by 1H NMR spectra.","PeriodicalId":9405,"journal":{"name":"Butlerov Communications","volume":"111 3S 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-10-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74805886","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2019-10-31DOI: 10.37952/roi-jbc-01/19-60-10-74
A. Lapin, M. Gordeeva, M. Kalaida
The article presents the results of a biochemical study of the total antioxidant activity of water during the Clarias gariepinus farming in closed containment aquaculture system, including the dynamics without replacement. For the first time is shown an increasing the total antioxidant activity with the highest values in the lower part of the biological filter. According to the results of daily observation, the fish behavior was adequate until the end of the experiment, which was stopped with the beginning of their mass death (more than 20%). Researches have shown the promise of using the indicator of total antioxidant activity to assess the work of the closed containment aquaculture system for hydrobionts farming. The issues of reducing the cost of farmed fish by the closed containment aquaculture system using aquaponics, which distinguished among other technologies by the high quality of environmentally friendly food products while significantly saving water resources which is an important problem for closed containment aquaculture system are considered. Food plants feed on bacteria from the waste products of fish while they consume the necessary secretion products from water – chemicals (nitrogenous, potassium, phosphorus compounds), naturally purifying the water. Aquaponics simulates the natural whirlpool, using the natural processes of fish vital functions for plants nutrient medium. As food plants can be used Salicornia europaea and glycophyte Nasturtium officinale, which has a high productivity and high content of vitamins, iron and glycosides. Both plants are tested in the closed containment aquaculture system including human, increased degree of isolation.
{"title":"Antioxidant properties of aqueous media. Part 3. Water research during the Clarias gariepinus farming in the closed containment aquaculture system","authors":"A. Lapin, M. Gordeeva, M. Kalaida","doi":"10.37952/roi-jbc-01/19-60-10-74","DOIUrl":"https://doi.org/10.37952/roi-jbc-01/19-60-10-74","url":null,"abstract":"The article presents the results of a biochemical study of the total antioxidant activity of water during the Clarias gariepinus farming in closed containment aquaculture system, including the dynamics without replacement. For the first time is shown an increasing the total antioxidant activity with the highest values in the lower part of the biological filter. According to the results of daily observation, the fish behavior was adequate until the end of the experiment, which was stopped with the beginning of their mass death (more than 20%). Researches have shown the promise of using the indicator of total antioxidant activity to assess the work of the closed containment aquaculture system for hydrobionts farming. The issues of reducing the cost of farmed fish by the closed containment aquaculture system using aquaponics, which distinguished among other technologies by the high quality of environmentally friendly food products while significantly saving water resources which is an important problem for closed containment aquaculture system are considered. Food plants feed on bacteria from the waste products of fish while they consume the necessary secretion products from water – chemicals (nitrogenous, potassium, phosphorus compounds), naturally purifying the water. Aquaponics simulates the natural whirlpool, using the natural processes of fish vital functions for plants nutrient medium. As food plants can be used Salicornia europaea and glycophyte Nasturtium officinale, which has a high productivity and high content of vitamins, iron and glycosides. Both plants are tested in the closed containment aquaculture system including human, increased degree of isolation.","PeriodicalId":9405,"journal":{"name":"Butlerov Communications","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-10-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83240212","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2019-09-30DOI: 10.37952/roi-jbc-01/19-59-9-93
D. D. Ziganshin, A. Sirotkin, Zlata A. Ostroumova, A. A. Egorshina, Mikhail A. Lukyantsev
The basic physical parameters of the cultivation of micromycete Trichoderma asperellum VKPM F-1323 are determined on complex nutrient media. The choice of the object of study was due to its antagonistic activity with attitude to many phytopathogenic fungi such as Ascochyta pisi, Cercospora beticola, Claviceps purpurea, Sclerotinia sclerotiorum, Alternaria alternata, Botrytis cinerea, Fusarium graminearum, Passalora fulva, Verticillum dahliae, as well as growth-stimulating activity with attitude to plants, suggesting a motivation for the use of Trichoderma asperellum VKPM F-1323 as the basis for biological products used in agriculture. During the experiment, the nutrient medium composition (g/l) was used: molasses – 20, yeast extract – 7, NaNO3 – 2, K2HPO4 – 1, KCl – 0.5, MgSO4 – 0.5, FeSO4 – 0.01. Before sterilization, the pH was adjusted to 7.5. Cultivation was carried out at a temperature of 27 °C with constant stirring and aeration in autoclaved laboratory fermenters with a working volume of 2 l. The cultivation of micromycete in a liquid nutrient medium was chosen in connection with the rapid progress of the process. In addition, unlike solid-phase cultivation, the deep one allows accumulating in the finished product form numerous secondary metabolites with antagonistic activity against phytopathogens, as well as growth-stimulating activity with attitude to plants. In the work, the values of mixing speed, aeration intensity, and initial pH of the medium are determined, which determine the maximum productivity of the process according to the conidia concentration (titer) of the studied culture. During the cultivation process, the pH level was monitored without maintaining it during the process, since it is known that a change in pH values characterizes the course of the cultivation process with the formation of spore forms, and the initial pH value is an important factor in the conidia formation of Trichoderma fungi. It is shown that during cultivation for 72 hours the maximum concentration of conidia is achieved for a stirring speed of 700 rpm, without reflective baffles (chippers) in the design of the fermenter, aeration intensity of 0.25 l/l of medium×min and the initial pH of the nutrient medium 7.0. Subject to the above conditions, the concentration of conidia is 1.35 ± 0.09 conidia /ml.
{"title":"Determination of the parameters of the submerged cultivation of micromycete Trichoderma asperellum VKPM F-1323 for obtaining spore forms of culture","authors":"D. D. Ziganshin, A. Sirotkin, Zlata A. Ostroumova, A. A. Egorshina, Mikhail A. Lukyantsev","doi":"10.37952/roi-jbc-01/19-59-9-93","DOIUrl":"https://doi.org/10.37952/roi-jbc-01/19-59-9-93","url":null,"abstract":"The basic physical parameters of the cultivation of micromycete Trichoderma asperellum VKPM F-1323 are determined on complex nutrient media. The choice of the object of study was due to its antagonistic activity with attitude to many phytopathogenic fungi such as Ascochyta pisi, Cercospora beticola, Claviceps purpurea, Sclerotinia sclerotiorum, Alternaria alternata, Botrytis cinerea, Fusarium graminearum, Passalora fulva, Verticillum dahliae, as well as growth-stimulating activity with attitude to plants, suggesting a motivation for the use of Trichoderma asperellum VKPM F-1323 as the basis for biological products used in agriculture. During the experiment, the nutrient medium composition (g/l) was used: molasses – 20, yeast extract – 7, NaNO3 – 2, K2HPO4 – 1, KCl – 0.5, MgSO4 – 0.5, FeSO4 – 0.01. Before sterilization, the pH was adjusted to 7.5. Cultivation was carried out at a temperature of 27 °C with constant stirring and aeration in autoclaved laboratory fermenters with a working volume of 2 l. The cultivation of micromycete in a liquid nutrient medium was chosen in connection with the rapid progress of the process. In addition, unlike solid-phase cultivation, the deep one allows accumulating in the finished product form numerous secondary metabolites with antagonistic activity against phytopathogens, as well as growth-stimulating activity with attitude to plants. In the work, the values of mixing speed, aeration intensity, and initial pH of the medium are determined, which determine the maximum productivity of the process according to the conidia concentration (titer) of the studied culture. During the cultivation process, the pH level was monitored without maintaining it during the process, since it is known that a change in pH values characterizes the course of the cultivation process with the formation of spore forms, and the initial pH value is an important factor in the conidia formation of Trichoderma fungi. It is shown that during cultivation for 72 hours the maximum concentration of conidia is achieved for a stirring speed of 700 rpm, without reflective baffles (chippers) in the design of the fermenter, aeration intensity of 0.25 l/l of medium×min and the initial pH of the nutrient medium 7.0. Subject to the above conditions, the concentration of conidia is 1.35 ± 0.09 conidia /ml.","PeriodicalId":9405,"journal":{"name":"Butlerov Communications","volume":"31 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75077546","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2019-09-30DOI: 10.37952/roi-jbc-01/19-59-9-71
A. I. Fokina, V. Kulakov, Elena A. Klekovkina, T. Ashikhmina
Inverse voltammetry is a very perspective method due to its relative simplicity, cost effectiveness, and sensibility. Universality of this method allows scientists to find new objectives, both organic and inorganic nature, for the use of the method. Some results of the improvement and adaptation of the standardized methodology for cobalt identification with a rotating disk electrode implemented on the analyzer «Ecotest-VA» with the «ЕМ-04» module for the identification of the mass concentration of this metal in the medication «Cyanocobalamin» is presented in this article. The arrival of an analytical signal in the form of peaks on a voltamperogram during the quantitative determination of cobalt results from the adsorptive concentration of cobalt-dimethylglyoxime complexes on the surface of the working cathode. Cathode current registered when Еmax = (-1.1)–(-1.2) V is compliant with catalytic current of electrochemical reduction of hydrogen from adsorbed cobalt dimethylglyoxime and is an analytical signal of a measured ion, in the present case – of cobalt. Peak height (area) is proportional to the metal-ion concentration in the solution. It is necessary to carry out the sample preparation of the medication and a solution for additive components for the implementation of the analysis method when determining the mass concentration of the metal in the cyanocobalamin solution. The cyanocobalamin solution with the addition of hydrogen peroxide is maintained in a photolysis camera for the transportation of cobalt into the solution as a Со3+. The solution for additive components is boiled with hydrogen peroxide to convert Со2+ into Со3+. Using the developed method, the evaluation of cobalt in the medication «Cyanocobalamin» (0.5 mg/сm3) was conducted. Validation of the results obtained was carried out with the use of the technique «entered-identified».
{"title":"Evaluation of cobalt in the cyanocobalamin solution using the method of inverse voltammetry with a rotating disk electrode","authors":"A. I. Fokina, V. Kulakov, Elena A. Klekovkina, T. Ashikhmina","doi":"10.37952/roi-jbc-01/19-59-9-71","DOIUrl":"https://doi.org/10.37952/roi-jbc-01/19-59-9-71","url":null,"abstract":"Inverse voltammetry is a very perspective method due to its relative simplicity, cost effectiveness, and sensibility. Universality of this method allows scientists to find new objectives, both organic and inorganic nature, for the use of the method. Some results of the improvement and adaptation of the standardized methodology for cobalt identification with a rotating disk electrode implemented on the analyzer «Ecotest-VA» with the «ЕМ-04» module for the identification of the mass concentration of this metal in the medication «Cyanocobalamin» is presented in this article. The arrival of an analytical signal in the form of peaks on a voltamperogram during the quantitative determination of cobalt results from the adsorptive concentration of cobalt-dimethylglyoxime complexes on the surface of the working cathode. Cathode current registered when Еmax = (-1.1)–(-1.2) V is compliant with catalytic current of electrochemical reduction of hydrogen from adsorbed cobalt dimethylglyoxime and is an analytical signal of a measured ion, in the present case – of cobalt. Peak height (area) is proportional to the metal-ion concentration in the solution. It is necessary to carry out the sample preparation of the medication and a solution for additive components for the implementation of the analysis method when determining the mass concentration of the metal in the cyanocobalamin solution. The cyanocobalamin solution with the addition of hydrogen peroxide is maintained in a photolysis camera for the transportation of cobalt into the solution as a Со3+. The solution for additive components is boiled with hydrogen peroxide to convert Со2+ into Со3+. Using the developed method, the evaluation of cobalt in the medication «Cyanocobalamin» (0.5 mg/сm3) was conducted. Validation of the results obtained was carried out with the use of the technique «entered-identified».","PeriodicalId":9405,"journal":{"name":"Butlerov Communications","volume":"250 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74505642","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
京公网安备 11010802042870号
京ICP备2023020795号-1
扫码关注我们
求助内容：
应助结果提醒方式：