scholarly journals SYNTHESIS OF NOVEL 4-R-1,2,4-TRIAZOLIN-5-THIONES CONTAINING SPACE-HINDERED FRAGMENT OF PHENOL

Author(s):  
Vladimir N. Koshelev ◽  
Ludmila V. Ivanova ◽  
Rahman T.Kh. Alasadi ◽  
Olga V. Primerova

Using of additives inhibiting free radical processes is necessary at production of the lubricating oils. In given article such kind target compounds were obtained from the number of new 1-acyl-4-R-thiosemicarbazides which were synthesized on the base of 3- (4-hydroxy-3,5-di-tert-butyl) propanoic acid hydrazide. The starting hydrazide was prepared from commercially available methyl ester (methylox) by refluxing in ethanol with a slight excess of hydrazine hydrate for 8 h. The best yields of the 1-acyl-4-R-isothiocyanates were achieved by refluxing equimolar amounts of isothiocyanates and hydrazide in isopropanol for 4-5 h. Under these conditions the yield was 75-85%. At further cyclization of intermediates obtained at a first step in aqueous sodium hydroxide for 1.5 h the corresponding 3-acyl-4-R-1,2,4-triazolin-5-thiones were obtained with the yield of 70-90%. Also, this method has absolute advantages due to a simple isolation of target compounds. Based on the IR-spectroscopy data in middle region and 1H NMR spectroscopy it was established that the substances obtained in the crystalline state and in DMSO solution exist in a form of thiones. The composition of obtained substances was determined with elemental analysis whereas the structures of the synthesized compounds were confirmed with FT-IR spectroscopy methods, 1H NMR spectroscopy and mass spectrometry.Forcitation:Koshelev V.N., Ivanova L.V., Alasadi R.T.Kh., Primerova O.V. Synthesis of novel 4-R-1,2,4-triazolin-5-thiones containing space-hindered fragment of phenol. Izv. Vyssh. Uchebn. Zaved. Khim. Khim. Tekhnol. 2017. V. 60. N 3. P. 43-47.

2013 ◽  
Vol 10 (3) ◽  
pp. 818-827
Author(s):  
Baghdad Science Journal

A series of new compounds including p-bromo methyl pheno acetate [2]. N-( aminocarbonyl)–p-bromo pheno acetamide [3] , N-( aminothioyl) -p-bromo phenoacetyl amide [4], N-[4-(p-di phenyl)-1,3-oxazol-2-yl]-p-bromopheno acetamide [5],N-[4-p-di phenyl]-1,3-thiazol-2-yl-p-bromo phenoacet amide [6], p-bromopheno acetic acid hydrazide [7] , 1-N-(p-bromo pheno acetyl)-1,2-dihydro-pyridazin-3,6- dione [8], 1-N-(p-bromo pheno acetyl)-1,2-dihydro-phthalazin-3,8- dione[ 9], 1-(p-bromo pheno acetyl)-3-methylpyrazol-5-one [10] and 1-(p-bromo phenol acetyl)- 3,5-dimethyl pyrazole [11] have been synthesized. The prepared compounds were characterized by m.p.,FT-IR and 1H-NMR spectroscopy. Also ,the biological activity was evaluated .


2017 ◽  
Author(s):  
◽  
Sharista Raghunath

The presence of dyes in effluent poses various environmental as well as health hazards for many organisms. Although various remediation strategies have been implemented to reduce their effect, dyes still manage to infiltrate into the environment and hence new strategies are required to address some of the problems. This study investigated the innovation of two cationic water-soluble polymers viz., Proline-Epichlorohydrin-Ethylenediamine Polymer (PEP) and Thiazolidine-Epichlorohydrin-Ethylenediamine Polymer (TEP) that were used to remediate selected synthetic dyes from synthetic effluent by adsorption and dye reduction. Both polymers were synthesized using monomers of a secondary amine, epichlorohydrin and ethylenediamine and were subsequently characterized and modified and their remediation potential studied. In the first study, PEP was synthesized and characterized by 1H-NMR Spectroscopy, FT-IR Spectroscopy, dynamic light scattering, and thermogravimetric analysis (TGA). Thereafter PEP was modified with bentonite clay, by simple mixing of the reactants, to form a Proline-Epichlorohydrin-Ethylenediamine Polymer-bentonite composite (PRO-BEN); it was characterized by FT-IR Spectroscopy, scanning electron microscopy (SEM)/ energy dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Adsorption studies were then undertaken with a synthetic effluent containing three textile dyes, viz., Reactive Blue 222 (RB 222), Reactive Red 195 (RR 195) and Reactive Yellow (RY 145). Various conditions were investigated including pH of the solution, temperature, sodium chloride concentration, initial dye concentration and the dosage of adsorbent used. The experimental data for all dyes followed a Langmuir isotherm. The adsorption process was found to be pseudo-second order. According to the thermodynamic parameters, the adsorption of the dyes was classified as physisorption and the reaction was spontaneous and exothermic. The data were also compared using studies with alumina as an adsorbent. Results showed that PRO-BEN exhibited better absorptivity and desorption than alumina making its use a better recyclable remediation strategy for the removal of organic dyes in wastewater treatment plants. In the second study, TEP was synthesized and then characterized by FT-IR Spectroscopy, 1H-NMR Spectroscopy, TGA and DLS. Thereafter, TEP was used to prepare TEP capped gold nanoparticles (TEP-AuNPs). Herein, two methods were investigated: the Turkevich method and an adaptation of the Turkevich method using bagasse extract. The TEP-AuNPs was characterized by FT-IR Spectroscopy, SEM, EDX, DLS and TEM. Thereafter the reduction of each of Allura Red, Congo Red and Methylene Blue was investigated with the TEP-AuNPs for its catalytic activity toward dye reduction. This study showed that the batch of AuNPs prepared by the Turkevich method had higher rates of dye reduction compared with AuNPs prepared using bagasse extract. Also the quantity of TEP used as capping agent greatly influenced the size, shape and surface charge of the nanoparticles as well as their catalytic performance: the Vroman effect explained this behavior of the TEP-AuNPs. It was finally concluded that whilst PRO-BEN, in the first study, showed excellent dye remediation properties, the second study on TEP-AuNPs showed good catalytic activity for the reduction of selected dyes, however, it was more effective at lower polymer concentration. Finally, both materials displayed good potential for the clean-up of selected synthetic dyes from synthetic effluents.


2012 ◽  
Vol 50 (2) ◽  
pp. 148-158 ◽  
Author(s):  
A. Baglieri ◽  
M. Gennari ◽  
A. Ioppolo ◽  
P. Leinweber ◽  
M. Nègre

2002 ◽  
Vol 78 (4) ◽  
pp. 205-215 ◽  
Author(s):  
N Kovac ◽  
O Bajt ◽  
J Faganeli ◽  
B Sket ◽  
B Orel

Molbank ◽  
10.3390/m1261 ◽  
2021 ◽  
Vol 2021 (3) ◽  
pp. M1261
Author(s):  
Shintaro Kodama ◽  
Kazuki Bunno ◽  
Akihiro Nomoto ◽  
Akiya Ogawa

4,4′-di-tert-butyl-2,2′-bipyridinium trifluoromethanesulfonate was synthesized by stirring 4,4′-di-tert-butyl-2,2′-bipyridine with scandium(III) trifluoromethanesulfonate in acetonitrile, followed by precipitation with diethyl ether. The structure of the new compound was characterized by FT-IR, 1H, 13C{1H} and 19F{1H} NMR spectroscopy and CHN elemental analysis. This is a safe and simple method to obtain mono-protonated bipyridinium trifluoromethanesulfonate without the direct use of trifluoromethanesulfonic acid.


Author(s):  
Michael-Hannes Hoffelner ◽  
Werner Seebacher ◽  
Marcel Kaiser ◽  
Pascal Mäser ◽  
Eva-Maria Pferschy-Wenzig ◽  
...  

AbstractThe reaction of 2,3-dihydropyridines with sulfonyl halides surprisingly yielded open chain dienes with sulfonylimine structure. The products were specific out of several possible isomers and, therefore, a separation of isomers was not necessary. All new compounds were characterized using FT-IR spectroscopy, HRMS, and NMR spectroscopy. A bicyclic by-product from the reaction of a 2,3-dihydropyridine with mesyl chloride was isolated and its structure elucidated using a single X-ray crystal analysis. Some biological activities, like antimicrobial and cytotoxic properties were investigated. Graphic abstract


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