{"title":"ALKYLATION OF 3-FORMYLQUINOLINE-2-ONE WITH ALKENYL(ALKYNYL) BROMIDES","authors":"T. Sabo, M. Onysko","doi":"10.24144/2414-0260.2024.1.76-81","DOIUrl":"https://doi.org/10.24144/2414-0260.2024.1.76-81","url":null,"abstract":"Functional and condensed quinolin-2-one derivatives exhibit a wide range of biological activity. The presence of an aldehyde group and modification at position 1 or 2 of quinolin-2-one expand the searching for new biologically active compounds. One of the directions of such modification is the annulation of an additional azaheterocycle to quinoline. In this work, the interaction of unsaturated alkyl halides (4-bromobut-1-ene, 5-bromopent-1-ene, 5-bromopent-1-yne) with 3-formylquinolin-2-one was investigated. The reaction was carried out in the presence of dimethylformamide using sodium hydride at room temperature or heating to 80°C for 8 hours. It was shown that under the found conditions, non-regioselective alkylation occurs with the formation of a mixture of O- and N-alkylation isomers. According to spectral data, the ratio of alkylation products depends on the alkylating agent. Thus, in case of using 3-formylquinolin-2-one, 4-bromobut-1-ene or 5-bromopent-1-yne, a mixture of O- and N-alkyl quinolines is formed in a ratio of 1:1.5, and in case of 5-bromopent-1-ene - 2:1. N-butenyl-3-formylquinolin-2-one was isolated by fractional crystallization, and in other cases, mixtures with minor amounts of one of the isomers were isolated.","PeriodicalId":437217,"journal":{"name":"Scientific Bulletin of the Uzhhorod University. Series «Chemistry»","volume":"65 12","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141652508","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}
{"title":"RESEARCH OF THE TETRARY COMPOUND Tb1-xNaxSn2 (x = 0,1) BY SINGLE CRYSTAL METHOD","authors":"A. Stetskiv, V. Pavlyuk","doi":"10.24144/2414-0260.2024.1.44-53","DOIUrl":"https://doi.org/10.24144/2414-0260.2024.1.44-53","url":null,"abstract":"The crystal structure of the ternary phase Tb1-xNaxSn2 (x = 0,1) (a = 0,4412(1), b = 1,6314(2), c = 0,4314(1) nm), which belongs to the ZrSi2, просторова група, символ Пірсона) structure type (space group Cmcm, Pearson symbol oS12), was investigated by single crystal method using single crystal diffractometer XCALIBUR (Mo Ka-radiation). This structure was resolved by means direct method. Atomic and thermal displacement parameters are refined by SHELX-97.\u0000For the synthesis of alloys with sodium, pieces of pure metals with a certain stoichiometric composition were pressed into tablets, which were placed in a tantalum crucible and placed in a resistance furnace with a temperature controller. The rate of heating from room temperature to 400 ºС was equal to 5 ºС per minute. At this temperature, the alloys were kept for two days, and then the temperature was increased from 400 ºС to 800 ºС for 1 hour. The obtained samples were annealed at the same temperature for 8 hours. The alloys were stored under a layer of indifferent oil, previously cleaned and dehydrated. Homogenizing annealing was carried out at a temperature of 200 °C for 480 hours.\u0000The results of calculation and refinement of the crystal structure of compound Tb1-xNaxSn2 (x = 0,1) shown, that it is isostructural to the structural type ZrSi2, where Tb(Na) atoms form a statistical mixture and occupy the positions of Zr atoms, and Sn1 and Sn2 atoms occupy the positions of Si2 and Si1 atoms respectively.\u0000The number of neighboring atoms correlates well with the size of the central atoms. The largest atoms of a rare earth metal (Tb) or an alkali metal (Na) when forming a statistical mixture are characterized by a coordination number of 10 and their atoms are arranged in the form of a distorted four-capped trigonal prism. The coordination polyhedron for the Sn1 atom is a double antitrigonal prism. For other tin atoms (Sn2), the coordination polyhedron in this structure is a trigonal prism. The shortest interatomic distances are typical for intermetallic compounds and their values indicate the metallic type of bond.","PeriodicalId":437217,"journal":{"name":"Scientific Bulletin of the Uzhhorod University. Series «Chemistry»","volume":"45 5","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141654767","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}
{"title":"COMPLEXES OF TELLURIUM TETRAHALIDES WITH 3-ALLYL-2-(2-METHYLTHIO)QUINAZOLIN-4(3H)-ONE","authors":"D.Yu. Kulia, D. Kut, M. Kut, M. Onysko","doi":"10.24144/2414-0260.2024.1.70-75","DOIUrl":"https://doi.org/10.24144/2414-0260.2024.1.70-75","url":null,"abstract":"Regioselectivity in organic chemistry is a crucial concept for the synthesis of organic heterocyclic compounds. This concept determines the direction of a reaction towards the formation of a specific product from a possible set of structures. In this context, the regioselectivity of electrophilic heterocyclization depends on the nature of the electrophilic reagent, the structure of the substrate, and the polarity of the solvent. Special attention is given to substrates with two unsaturated fragments. Literature data have shown that the reaction depends on the type of electrophilic reagent; for example, iodination leads to the annulation of a six-membered dihydrothiazine, while bromination results in the annulation of a thiazolinone ring.\u0000In this study, the interaction of tellurium tetrahalides with 3-allyl-2-(2-methylthio)quinazolin-4(3H)-one, which has various alkene substituents, was investigated. Prior to the study, the initial metallothioether was synthesized for the first time.\u0000In the reaction of tellurium tetrahalides with 3-allyl-2-(2-methylthio)quinazolin-4(3H)-one, molecular adducts of thioether-tellurium tetrahalide with a 1:1 ratio were obtained. The experimental results demonstrate that an excess of the halogenating reagent and changes in reaction conditions do not affect the reaction product.\u0000Thus, this work highlights the importance of studying the regioselectivity of electrophilic intramolecular heterocyclization reactions and the potential use of tellurium tetrahalides for obtaining molecular complexes.","PeriodicalId":437217,"journal":{"name":"Scientific Bulletin of the Uzhhorod University. Series «Chemistry»","volume":"9 6","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141653554","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}
{"title":"Kut D., Kut M., Onysko M., Lendel V. STUDY OF REGIO- AND STEREO-SELECTIVITY OF HALOGEN-INDUCED CYCLIZATION OF TERMINAL PROPARGYL THIOETHERS OF 3-ALKYL(PHENYL)QUINAZOLINE-4-ONES","authors":"D. Kut, M. Kut, M. Onysko, V. Lendel","doi":"10.24144/2414-0260.2023.2.46-52","DOIUrl":"https://doi.org/10.24144/2414-0260.2023.2.46-52","url":null,"abstract":"Polycyclic condensed quinazoline derivatives are biologically valuable compounds that have found their application in pharmaceutical and medicinal chemistry. Their practical use makes such compounds interesting and promising, and their synthesis is an urgent task. In the present work, the regio- and stereo-selectivity of the halocyclic reaction of propargyl thioethers of 2-thioxoquinazoline-4-one with bromine, iodine and iodine bromide, the effect of solvent polarity, acceptor substituent at position 7 of quinazoline, and the steric effect of the substituent at N(3) of quinazoline on the course of the electrophilic heterocyclic reaction were investigated. It was found that the halogenation of 3-alkyl-2-thioxo-2,3-dihydroquinazoline-4(1H)-ones in chloroform or ice-cold acetic acid proceeds regio- and stereo-selectively with the formation of salt-like thiazoloquinazoline halides. On the contrary, the stereoselectivity of halogenation of the 3-phenyl substituted propargyl thioether of quinazoline depends on the polarity of the solvent and in chloroform leads to the formation of a mixture of configurational isomers of thiazoloquinazoline tribromide, while in acetic acid, presumably, one geometric isomer is formed. The structure of the obtained polycyclic systems was proved on the basis of NMR spectroscopy and elemental analysis. \u0000Keywords: propargyl thioethers; halogenation; stereo-selectivity; regio-selectivity; thiazoloquinazoline halides.","PeriodicalId":437217,"journal":{"name":"Scientific Bulletin of the Uzhhorod University. Series «Chemistry»","volume":"232 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-01-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140500308","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}
{"title":"Sidey V.I. ON THE IONIC RADIUS OF THE CYANIDE ION","authors":"V. Sidey","doi":"10.24144/2414-0260.2023.2.11-15","DOIUrl":"https://doi.org/10.24144/2414-0260.2023.2.11-15","url":null,"abstract":"In a number of crystal structures, the linear two-atom cyanide ion CN– is capable of exhibiting orientational disorder and thus can be considered as a spherical anion similar to halide ions. The aim of this work was to determine the value of the octahedral (i.e., assigned to the standard crystallochemical coordination number CN = 6, which corresponds to the octahedral surroundings of the central atom of the coordination sphere by ligands) effective ionic radius and the corresponding crystal radius for the orientationally disordered cyanide ion by using the Shannon methodology [Shannon R.D. Acta Crystallogr. 1976, A32(5), 751–767]. Using a modified Shannon’s approach based on the study of a series of correlation dependences (constructed for a number of isostructural analogous compounds with a common cation) between the cube of the effective ionic radius r3 of the anion and the volume V of the unit cell of the relevant crystal structure, the octahedral effective ionic radius of the cyanide ion was determined to be ~1.935 Å. Calculated in accordance with the Shannon’s rule, the crystal octahedral radius (i.e., the effective ionic radius of the anion reduced by a constant value of 0.14 Å) for the cyanide ion is ~1.795 Å. The obtained values of the octahedral radii of the cyanide ion are compatible with the Shannon system of effective ionic radii and crystal radii, and thus can be used along with the original Shannon radii to model crystal structures containing orientationally disordered cyanide ions. \u0000Keywords: cyanide ion; ionic radius; orientational disorder; crystal structure.","PeriodicalId":437217,"journal":{"name":"Scientific Bulletin of the Uzhhorod University. Series «Chemistry»","volume":"326 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-01-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140500999","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}
{"title":"Selezen А.О., Piskach L.V. INTERACTION IN THE QUASI-TERNARY Tl2Se–CdSe–SnSe2 SYSTEM","authors":"A. O. Selezen, L. Piskach","doi":"10.24144/2414-0260.2023.2.16-26","DOIUrl":"https://doi.org/10.24144/2414-0260.2023.2.16-26","url":null,"abstract":"The nature of physicochemical interaction in the Tl2Se–CdSe–SnSe2 system was investigated by X-ray diffraction, DTA and microstructure methods. The system at 570 K contains α-, β-, γ-, δ-, ε-, h-, σ-solid solution ranges of Tl2Se, CdSe, SnSe2, Tl4SnSe4, Tl2SnSe3, Tl2Sn2Se5 and a low-temperature modification of the quaternary compound Tl2CdSnSe4 that crystallizes in the tetragonal SG I-42m. The liquidus surface projection of this system includes the fields of the primary crystallization of all solid solutions, and h¢-solid solution ranges of HT-modification of Tl2CdSnSe4. These fields are separated by 21 monovariant curves and 19 nonvariant points. Six nonvariant processes occur in this system: three peritectic LU1+β↔d+σ, LU2+β↔σ¢+γ, LU3+γ↔ σ¢+h and three eutectic LE1↔α+β+d, LE2↔δ+ε+σ, LE3↔ε+h+σ and the processes associated with the phase transition of the quaternary phase σ↔σ¢. Two quasi-binary sections Tl4SnSe4–CdSe and Tl2SnSe3–CdSe triangulate the quasi-ternary Tl2Se–CdSe–SnSe2 system into three subsystems, Tl2Se–CdSe–Tl4SnSe4, Tl4SnSe4–CdSe–Tl2SnSe3, and Tl2SnSe3–CdSe–SnSe2, for which spatial state diagrams were plotted. The eutectic process E1 takes place in the first subsystem at 592 K; the second subsystem features peritectic process U1 at 680 K and eutectic process E2 at 665 K. Two peritectic processes U2 at 775 K and U3 at 696 K and the eutectic process E3 at 643 K take place in the third subsystem; the plane at 623 K is associated with the solid-phase decomposition of the Tl2Sn2Se5 compound by reaction h↔ε+γ. \u0000Keywords: phase equilibria; polythermal sections; liquidus surface; spatial state diagrams.","PeriodicalId":437217,"journal":{"name":"Scientific Bulletin of the Uzhhorod University. Series «Chemistry»","volume":"375 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-01-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140501067","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}
N. Golub, E.O. Holub, A. Kozma, H. F. Hlebena, H.M. Mykhalchuk, A.O. Kuznyetsova
{"title":"Golub N.P., Golub E.O., Kozma A.A., Hlebena H.F., Mikhalchuk H.M., Kuznietsova A.O. SYNTHESIS AND RESEARCH OF A COMPLEX MANGANESE-NICKELPHOSPHATE CATALYTIC SYSTEM","authors":"N. Golub, E.O. Holub, A. Kozma, H. F. Hlebena, H.M. Mykhalchuk, A.O. Kuznyetsova","doi":"10.24144/2414-0260.2023.2.53-61","DOIUrl":"https://doi.org/10.24144/2414-0260.2023.2.53-61","url":null,"abstract":"Individual Mn2P2O7 and Ni3(PO4)2 phosphate catalysts were synthesized. A new synthesis technique was developed and a new complex catalytic system хMn2P2O7×yNi3(PO4)2 was obtained based on them (К-1 – К-7), which has the predicted physicochemical properties. The composition of these phosphates in the structure of the catalyst was varied in the range of 0,5 – 99,5 wt.%. It was established that the conditions of synthesis of catalysts significantly influence the process of forming the composition, structure, and corresponding physicochemical parameters of the synthesized catalysts. On the thermogram of the differential thermal analysis of an individual manganese-phosphate catalyst, three endo-effects at 148°С, 220°С and 353°С and one exo-effect at 460°С are observed. The thermogram of individual Ni3(PO4)2 shows two endo-effects at 210°С and 372°С and one exo-effect at 803°С. The synthesized double manganese-containing systems are characterized by a significant difference in DTA curves for samples K-1 - K-7. All obtained air-dry samples are crystal hydras with different numbers of water molecules. The structure of the obtained series of complex manganese-nickel phosphate catalysts contains various forms of water. The process of dehydration contributes to its separation from the structure of the samples and leads to the occurrence of characteristic endothermic effects. On all synthesized complex samples, the transition of manganese (II) orthophosphate to its pyrophosphate is observed when the final heat treatment temperature is reached. Firing samples of synthesized catalysts above 700oC leads to their complete dehydration with the formation of anhydrous salts. DTA results for all synthesized manganese-nickel phosphate samples are in good agreement with their X-ray diffraction, IR spectroscopy, and surface acidity results. They confirmed the correct choice of the modifying ion to improve the structure and physicochemical parameters of the manganese (II) phosphate catalyst. It can be predicted that the synthesized new complex oxide catalysts will show improved catalytic properties (activity and selectivity) in the processes of partial oxidation of n-alkanes into valuable products. The synthesized double manganese-containing systems are characterized by a significant difference in DTA curves for samples K-1 - K-7. All obtained air-dry samples are crystal hydras with different numbers of water molecules. The structure of the obtained series of complex manganese-nickel phosphate catalysts contains various forms of water. The process of dehydration contributes to its separation from the structure of the samples and leads to the occurrence of characteristic endothermic effects. On all synthesized complex samples, the transition of manganese (II) orthophosphate to its pyrophosphate is observed when the final heat treatment temperature is reached. Firing samples of synthesized catalysts above 700oC leads to their complete dehydration with the formation of an","PeriodicalId":437217,"journal":{"name":"Scientific Bulletin of the Uzhhorod University. Series «Chemistry»","volume":"280 12","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-01-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140499888","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}
O. Symkanych, O. Kokhan, O. Glukh, K. Krch, O. Lytvyn, N. Svatiuk, I.V. Butsyak
{"title":"Symkanych О.І., Коkhan О.P., Glukh О.S., Krch K.L., Lytvyn О.V., Svatiuk N.І., Butsyak І.V. MONITORING OF RADIONUCLIDE MIGRATION IN THE BOTTOM SEDIMENTS OF THE TISA BILA RIVER' SOURCE","authors":"O. Symkanych, O. Kokhan, O. Glukh, K. Krch, O. Lytvyn, N. Svatiuk, I.V. Butsyak","doi":"10.24144/2414-0260.2023.2.75-82","DOIUrl":"https://doi.org/10.24144/2414-0260.2023.2.75-82","url":null,"abstract":"The regularities of distribution, migration, and accumulation of natural gamma-active nuclides 40K, uranium 238U (214Pb, 214Bi), and thorium 232Th (212Pb, 212Bi, 228Ac, 208Tl) series, as well as man-made 137Cs in the sediments of the tributary of the Tysa River (Bila Tysa), have been established. It is shown that the total content of the studied radionuclides in the bottom sediments along the entire length of the Tysa River differs slightly and is proportional to the level of its siltation. And this largely depends on many factors, in particular - the intensity of radionuclide exchange processes between soil and water, the water content in the soil, organic substances, and the morphological features of the river. Fluctuations of the total specific activity of natural gamma-active radionuclides (excluding 40K) in sediments within the range of 195.5-293.9 Bq/kg were established. The highest content of these isotopes was determined at the confluence of the White and Black Tisza. Mapping of the studied territories according to the content of 40K and 137Cs has show that the area of accumulation of gamma-active nuclides is concentrated in the lower part of the river (the point of confluence of the White and Black Tisza), and the probable causes of this phenomenon were substantiated. The analysis of the degree of connection between the content of radionuclides (238U and 232Th, 40K and 137Cs series) and the territorial factor showed that for the majority of GAN there is a zonal distribution - in the bottom sediments of the river source. \u0000Keywords: radionuclides; gamma-active nuclides; radioecological monitoring; bottom deposits; migration; accumulation; Cs/K content; Tysa river.","PeriodicalId":437217,"journal":{"name":"Scientific Bulletin of the Uzhhorod University. Series «Chemistry»","volume":"5 8","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-01-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140499425","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}
{"title":"CONVERSION OF PROPANE TO FORMALDEHYDE ON IRON PHOSPHATE","authors":"V. Dzyamko","doi":"10.24144/2414-0260.2022.2.116-121","DOIUrl":"https://doi.org/10.24144/2414-0260.2022.2.116-121","url":null,"abstract":"Phosphates represent diverse complex systems, whose basic structural unit is tetrahedron. They are widely applied as catalysts, carriers of catalytic active substances, adsorbents and ion exchangers. Phosphoric acid and phosphates act as catalyst for reactions of alkylation, cracking, izomerization, polymerization, hydrogenation and dehydrogenation. Phosphates of some metals promote oxidation of normal alkanes with derivation of aldehydes, acids, spirits and maleic anhydride. \u0000The process of propane and propylene oxidation on iron phosphate is investigated, as well as the influence of such factors as temperature, contact time of the reacting mixture with the catalyst t, the ratio of oxygen and hydrocarbon concentration in a mixture, and the influence of hydrogen concentration on the given process is shown. \u0000It is demonstrated that the optimum conditions for the realization of propane oxidation process is the temperature of 973 K and t = 0.17 s. It is established that with excess propane in the reaction mixture propylene is the predecessor of formaldehyde. On the contrary, at small concentration of propane in the mixture formaldehyde will be derived immediately from propane. The schemes of propane and propylene oxidation in formaldehyde are offered. \u0000Keywords: catalyst; oxidatio; рhosphates; propane; propylene; formaldehyde.","PeriodicalId":437217,"journal":{"name":"Scientific Bulletin of the Uzhhorod University. Series «Chemistry»","volume":"5 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-05-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"115262953","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}
{"title":"ELABORATION OF CHEMICAL SENSOR SENSITIVE TO BORON BENZILATE","authors":"M. Fershal, N. Chubirka","doi":"10.24144/2414-0260.2022.2.43-53","DOIUrl":"https://doi.org/10.24144/2414-0260.2022.2.43-53","url":null,"abstract":"Over the last decades, the development of simple and selective methods for the determination of organic analytes has been getting attention from analytical chemists. Particularly, the same applies to biologically active substances of natural and artificial origin, precursors, and metabolites of pharmaceuticals[1]. An example of such substance is benzylic acid (2, 2-diphenyl-2-hydroxyacetic acid) (BA), gravimetric reagent for zirconium [2], a product of hydrolysis and a metabolite of the antispasmodic and sedative drugs Pipoxolan, Benactyzine, or Metacin [3]. The complexes of BA have been proposed as corrosion inhibitors for some steels and aluminum alloys [4]. Its derivatives are being studied as new analgesics [5], anticancer drugs [6], and also as deep eutectic solvents [7]. The BA was used in the synthesis of the psychotropic combatant substance 3-quinuclidinyl benzilate (BZ), which causes mental slowing, and hydrolyzes to form BC [8-11]. For BA determination high-performance liquid chromatography and chromatography-mass spectrometry [12-15] are mostly used, hence the development of simple methods for determining benzylic acid is pertinent and relevant. \u0000Boric acid is known to form compounds with diols, α-hydroxy acids, dicarboxylic acids, and α-diketones [16] and that was used in developing potentiometric sensors for the determination of mandelic acid and vitamin C [17, 18]. As BA also forms complexes with boric acid and various metals [19, 20] the H3BO3 has been used in the present study as a reagent for obtaining boric acid benzilate ester - the analytical form of BA, as well as the ionic associate of its anion with tetraoctylammonium(TOA) as the active substance of a potentiometric PVC plasticized sensor sensitive to the mentioned above analytical form. The complex formation has been confirmed using IR spectroscopy. On the IR spectrum of BA, the absorption bands in the region of 3393. 69 cm-1 and 1715. 77 cm-1, which correspond to the vibrations of –ОН and >С=О groups, respectively have been detected [23]. At the same time, in the IR spectrum of the complex, the absorption band of –ОН groups in the region of 3300 - 3400 cm-1 was absent, that indicates their participation in the formation of ether bonds, additionally, the intensive bands of >C=O in the region of 1723. 41 cm-1 and 1742. 05 cm-1 has appeared. The ion pair of tetraoctylammonium cation with synthesized complex ion [B(Benz)2]- has been used as an active substance of the potentiometric sensor. The metrological and operational characteristics of the sensor and the optimal conditions of the analytical form obtaining have been systematically studied. The optimized composition of the sensitive PVC membrane was 0. 1% of IP, 33. 0% of PVC and 66. 9% of o-NFOE. For high yield [B(Benz)(ОН)2]--analytical form preparation the boiling of BA for 15 minutes in the medium of a buffer solution that consists of H3BO3 (sat.) - 0. 1 M NaOH - 0. 1 M H3PO4 with a pH of 5. 5 is needed. In optimal con","PeriodicalId":437217,"journal":{"name":"Scientific Bulletin of the Uzhhorod University. Series «Chemistry»","volume":"11 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-05-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"121440650","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}