Bimetallic Group 6 Tricarbonyls Triply-Bridged by Bis(phenylthio)alkane Bidentate Ligands

2010 ◽  
Vol 93-94 ◽  
pp. 13-16
Author(s):  
Khalil J. Asali

Reactions of the labile complex (Me3tach)M(CO)3 (Me3tach = 1,3,5-trimethyl-1,3,5-triazacyclohexane; M = W, Mo) with bis(phenylthio)alkanes ( = PhS(CH2)nSPh), (2:3 molar ratio) in CH2Cl2 as solvent (at 35 oC M = W, 0 oC M = Mo) afforded in good yields bimetallic tricarbonyl complexes triply- bridged by bis(phenylthio)alkanes of the type [M(CO)3]2(μ-PhS-(CH2)n-SPh)3 [n = 3 (a), 4 (b), 5 (c), 6 (d); M = W (1), Mo (2)]. These new triply-bridged complexes were characterized by 1H NMR, FT-IR and elemental analysis. Additionally, it has been observed that the thermodynamic stability of some of these new complexes in chlorinated hydrocarbons depends mainly on the nature of the metal center and varies in the order W >> Mo.

2019 ◽  
Vol 20 (1) ◽  
pp. 160
Author(s):  
Taghreed Mohy Al-Deen Musa ◽  
Mahmoud Najim Abid Aljibouri ◽  
Bayader Fadhil Abbas ◽  
Nahid Hasani

The present paper deals with the synthesis of cobalt(II), nickel(II), copper(II) and cadmium(II) complexes with two bidentate ligands, L1 (3-(quinoxaline-2-yl)-coumarin) and L2 (2-methylene-2H-chromene-3-(methyl carbonimidic)thioanhydride). The L1 ligand was prepared by treating w-bromo-3-acetylcoumarin with 1,2-phenylenediamine whereas the ligand L2 was prepared through substitution reaction ofw-bromo-3-acetylcoumarin with potassium thiocyanate in ethanol medium. The confirmation of the structures for L1 and L2 were done by (C.H.N.S.) elemental analysis, FT-IR, NMR and mass spectra. The metal complexes of cobalt(II), nickel(II), copper(II) and cadmium(II), with L1 and L2, were prepared and isolated in the solid state then characterized by (C.H.N.M) elemental analysis, proton and carbon-13 NMR, FT-IR and mass spectra. Furthermore, the thermal analysis (TG-DSC) for some complexes assisted us in the elucidation of the suggested structures of complexes and confirmed their thermal stability. The results obtained from elemental analysis, magnetic susceptibility and thermal analysis confirmed that all metal complexes were formed in 2:1 molar ratio of ligand to metal with octahedral structures except cadmium(II) complexes which were in a tetrahedron geometry with 1:1 mole ratio. The complexes are found to be soluble in DMF and DMSO. The results obtained from TG-DSC analysis revealed that the metal complexes were thermally stable with point decomposition over 350 °C. The DFT/TDDFT calculations were carried out to provide the electronic structures and spectra of the compounds.


Author(s):  
Y. Khatoon ◽  
M. Shaquiquzzaman ◽  
V. Singh ◽  
M. Sarafroz

A series of 2, 5-disubstituted - 1, 3, 4 oxadiazoles (4a-o) were synthesized on refluxing hydrazine carbothioamides with iodine and potassium iodide in ethanolic sodium hydroxide solution starting from methyl-3-amino-4-hydroxy benzoate via synthesis of an intermediate methyl-2-substitutedaryl-1, 3-benzoxazole-5-carboxylates and 2-substitutedaryl-1, 3-benzoxazole-5-carbohydrazides. The newly synthesized compounds were characterized on the basis of spectral (FT-IR, 1H-NMR, MS) and elemental analysis. All these compounds were screened for anticonvulsant activity using Maximal Electroshock (MES) and subcutaneous pentylenetetrazole (scPTZ) method. Anticonvulsant activity was shown by majority of the synthesized compounds when given i.p. to mice. Among the tested compounds 4e, 4j and 4o were considered to have potent anticonvulsant activity comparable to that of standard drugs Phenytoin and Carbamazepine. Compounds 4e, 4g, 4h, 4i, 4k and 4m passed the rota rod test successfully without any sign of neurological deficit.


2011 ◽  
Vol 228-229 ◽  
pp. 919-924 ◽  
Author(s):  
Feng Yuan Huang

Cellulose Stearate (CS) was synthesized by acylating microcrystalline cellulose (MCC) in homogeneous system with p-toluenesulfonyl chloride (Tos-Cl) and stearic acid (SA). The reactive conditions were discussed. The molar ratio of AGU:SA:Tos-Cl was the key factor which affected the degree of substitution (DS) of CS. In the present paper, CSs with DS ranging from 0.64 to 2.35 were prepared under mild condition. The structure of CS was characterized by FT-IR and 1H-NMR, and DS of CS was determined by traditional saponification method and 1H-NMR, respectively. The solubility of CS was also investigated; the results showed that the higher DS of CS was, the easier CS dissolved in organic solvents. The thermal analysis was measured with DSC, and the results indicated that the glass transition temperature (Tg) and the maximum temperature of thermal decomposition (Tmax) of CS were dependent on DS.


2012 ◽  
Vol 217-219 ◽  
pp. 1159-1165 ◽  
Author(s):  
Yang Yang Shi ◽  
Ming Bo Wu ◽  
Yu Wei Wang ◽  
Shi Bin Li

Ethylene tar (ET) was utilized as raw material, 1,4-benzenedimethanol and trioxane as crosslinking agent to prepare condensed poly-nuclear aromatic resin (COPNAR). FT-IR, 1H-NMR, TGA, elemental analysis, and improved Brown-Ladner calculation were systematically conducted for ET, COPNAR, and COPNAR/graphite composites prepared via graphite molding. The ET average molecular structure parameters were calculated using improved Brown-Ladner method, the crosslinking agent was found an important factor for the COPNAR synthesis, and the obtained COPNAR and CONPAR/graphite composites exhibited highly beneficial heat resistance.


2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Yasir Arafat ◽  
Saqib Ali ◽  
Saira Shahzadi ◽  
Muhammad Shahid

Heterobimetallic complexes of Zn(II) and Sn(IV) with sarcosine have been synthesized at room temperature under stirring conditions by the reaction of sarcosine and zinc acetate in 2 : 1 molar ratio followed by the stepwise addition of CS2and organotin(IV) halides, where R = Me,n-Bu, and Ph. The complexes were characterized by elemental analysis, FT-IR and NMR (1H,13C) spectroscopy. IR data showed that the ligand acts in a bidentate manner. NMR data revealed the four coordinate geometry in solution state.In vitroantimicrobial activities data showed that complexes (3) and (4) were effective against bacterial and fungal strains with few exceptions.


2020 ◽  
Vol 32 (4) ◽  
pp. 952-958
Author(s):  
Ananya Vishwakarma ◽  
S.K. Sengupta ◽  
O.P. Pandey

Europium(III) and Terbium(III) complexes of type [Eu(L)Cl(H2O)2] and [Tb(L)OAc(H2O)2] (H2L = thiosemicarbazone ligands derived from substituted thiosemicarbazide and benzil/diacetyl) were synthesized. The ligands and synthesized complexes were characterized on the basis of elemental analysis, FT-IR and 1H NMR and X-ray diffraction studies. Photo-physical properties such as excitation spectra, emission spectra and luminescence curves of complexes were investigated. The most intense peak of Eu3+ ion found at 618 nm attributed to 5D0 → 7F2 transition and peak of Tb3+ ion at 549 nm attributed to 5D4 →7F5 transition.


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.


2020 ◽  
Vol 17 ◽  
Author(s):  
Mehri Abdollahi fard ◽  
Mohammadreza Manafi ◽  
Manijeh Motevalian ◽  
Seyed Saied Homami

Abstract: In this paper, a novel series of 1-(alkyl)-3-(2-oxo-2H-chromenyloxy acetamido) methylpyridinium salts were syn-thesized in a simple and efficient way. The method showed to be facile and the compounds were obtained in high isolated yields. All the synthesized compounds were characterized by 1H NMR, 13C NMR, FT-IR, Mass and elemental analysis. AChE and BuChE inhibition activity of the synthesized compounds were evaluated and the results showed that, all the com-pounds were active in the inhibition of the mentioned enzymes. All the compounds were active in the inhibition of the two studied enzymes. Among all the compounds, the compound 6a (1.85 μM) and 6i (0.106 μM) showed the highest inhibition activity against AChE and BuChE, respectively. The kinetic study was performed to get more insight into the mechanism of action of the synthesized compounds. Docking studies were also performed to obtain the interactions between the synthe-sized compounds and the enzymes.


2012 ◽  
Vol 77 (11) ◽  
pp. 1589-1597 ◽  
Author(s):  
Maryam Lashanizadegan ◽  
Marzieh Sarkheil

The Schiff base ligand trans-N,N?-bis[2-pyridinecarboxylidene] cyclohexane-1,2-diamine (L) was synthesized. This ligand when stirred with 1 equiv of MCl2.xH2O (M = Cu, Co, Zn) in ethanol, undergoes partial hydrolysis of the imino bond and the result tridentate ligand (L') and immediately forms the complexes with N3 coordination sphere. The reactions of L with MCl2.xH2O (M = Cu, Co, Zn) in THF give complexes [ML]Cl2. The ligand (L), complexes [M(L')Cl]Cl and [ML]Cl2 were characterized by elemental analysis, UV-Vis, FT-IR, 1H NMR, GC/MS and luminescence properties. The 1H NMR spectra of the ligand and its diamagnetic complexes were recorded in CDCl3 and DMSO solvents, respectively. Obtained data confirm that the donor atoms N in ligand coordinated to the metal ions. The luminescence studies show ligands and their complexes display intraligand (?- ?


2012 ◽  
Vol 554-556 ◽  
pp. 1350-1356 ◽  
Author(s):  
Xia Zhang ◽  
Lin Li ◽  
Jian Rong Huang ◽  
Ling Chen ◽  
Xiao Xi Li ◽  
...  

Naringin esters are paid more attention in medical and functional food industry than naringin due to their higher stability and solubility in lipidic environments. Naringin palmitic acid esters were enzymatically synthesized with naringin and palmitic acid. The effects of solvent type, temperature, concentration and types of enzymes and the molar ratio of substrates on the conversion of naringin were investigated. Novozym 435 performed higher catalytic ability in tert-amyl alcohol in the esterification of naringin with palmitic acid. The conversion yield of naringin increased with the increase of temperature (30-70°C) and of the concentration of enzyme. The structure of the naringin palmitate was characterized by FT-IR, 1H-NMR and HPLC-MS. 1H-NMR spectroscopic analysis indicated the presence of an ester bond on the C-6 of the glucose moiety of naringin molecule.


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