scholarly journals Reactions of MoCl5 and MoO2Cl2 with 4-Phenylimidazole-2-thiol and 2-Thiazoline-2-thiol

2020 ◽  
Vol 36 (6) ◽  
pp. 1096-1102
Author(s):  
Deepika Rani
Keyword(s):  
Liquid Nitrogen ◽  
1H Nmr ◽  
Elemental Analysis ◽  
Room Temperature ◽  
Inert Atmosphere ◽  
Molar Ratios ◽  
Vacuum Line

Reactions of MoCl5/MoO2Cl2 with 4-phenylimidazole-2-thiol/2-thiazoline-2-thiol in CH3CN solvent in 1:1/1:2 molar ratios have been carried out at room temperature. Products obtained MoCl3(C9H7N2S)(CH3CN),[1]; MoCl2(C9H7N2S)(CH3CN), [2]; Mo2OCl4(C9H8N2S)2, [3] and Mo4O2Cl12(C9H7N2S)4, [4]; MoO2Cl3(C3H5NS2)2, [5] and Mo2O4Cl3(C3H5NS2)2, [6] have been analyzed and characterized by elemental analysis, FTIR, 1H NMR and LC-MS techniques. Compounds being moisture and air sensitive, these have been prepared in inert atmosphere using vacuum line and liquid nitrogen cooled traps. Fragments obtained in LC-MS spectra support the formulae derived.

scholarly journals Reactions of MoCl5 and MoO2Cl2 with 4-Phenylimidazole-2-Thiol and 2-Thiazoline-2-Thiol

2020 ◽  
Vol 36 (6) ◽  
pp. 1096-1102
Author(s):  
Deepika Rani ◽  
Gursharan Singh ◽  
Seema Sharma
Keyword(s):  
Liquid Nitrogen ◽  
1H Nmr ◽  
Elemental Analysis ◽  
Room Temperature ◽  
Inert Atmosphere ◽  
Molar Ratios ◽  
Vacuum Line

Reactions of MoCl5/MoO2Cl2 with 4-phenylimidazole-2-thiol/2-thiazoline-2-thiol in CH3CNsolvent in 1:1/1:2 molar ratios have been carried out at room temperature. Products obtained MoCl3(C9H7N2S)(CH3CN), [1];MoCl2(C9H7N2S)(CH3CN), [2]; Mo2OCl4(C9H8N2S)2, [3] and Mo4O2Cl12(C9H7N2S)4, [4]; MoO2Cl3(C3H5NS2)2, [5] and Mo2O4Cl3(C3H5NS2)2, [6] have been analyzed and characterizedby elemental analysis, FTIR, 1H NMR and LC-MS techniques. Compounds being moisture and air sensitive, these have been prepared in inert atmosphere using vacuum line and liquid nitrogen cooled traps. Fragments obtained in LC-MS spectra support the formulae derived.

scholarly journals Reactions of MoCl5 and MoO2Cl2 with Succinimide, 1, 4-Diaminobutane, 3-Methylpyridine, 1, 3-Diaminopropane, Pyrazole and 1- Methylpyrrolidine in Tetrahydrofuran

2021 ◽  
Vol 37 (3) ◽  
pp. 634-642
Author(s):  
Rakesh Kumar ◽  
Gursharan Singh
Keyword(s):  
Biological Activity ◽  
Transition Metals ◽  
1H Nmr ◽  
Elemental Analysis ◽  
13C Nmr ◽  
Inert Atmosphere ◽  
Biologically Active ◽  
Vacuum Line ◽  
Characterization Studies ◽  
Hydrolysis Of

It has been reported that molybdenum may extract oxygen from oxygen containing ligands. Oxo complexes of above bases with transition metals show numerous applications and are biologically active. So to study the biological activity of molybdenum complexes and to study oxo abstraction reactions by molybdenum, reactions of succinimide/1, 4-diaminobutane/3-methylpyridine/1, 3-diaminopropane/pyrazole/1-methylpyrrolidine with MoCl5/MoO2Cl2 have been carried out, in THF medium using equimolar/bimolar quantities of the ligand, at normal temperature. The products thus obtained are: Mo2O3Cl5(C4H5NO2)2(C4H8O)2, [1]; Mo2O2Cl2(C4H5NO2)2(C4H8O)2, [2]; MoO2Cl2(H2NCH2CH2CH2CH2NH2)2, [3]; Mo3Cl8(C6H7N)4(C4H8O)2, [4]; Mo3Cl6(C6H7N)6(C4H8O)6, [5]; MoO2Cl3(H2NCH2CH2CH2NH2)2, [6]; Mo2O4Cl4(C3H4N2)4, [7] and Mo2O6Cl8(C5H11N)4, [8]. There is oxygen abstraction by molybdenum during the reaction from the oxygen containing solvent THF. Formulations of these compounds were made and their properties were studied with FTIR(transmission mode), 1H NMR/13C NMR, microbiological studies, elemental analysis(Mo, Cl, C, H, N) and LC-MS. All preparations, separations and isolations were executed in vacuum line and inert atmosphere (dry nitrogen) to eliminate any oxidation/hydrolysis of products by air/moisture. The formulations proposed have been supported by the above characterization studies.

Syntheses and Investigation of Properties of New Ionic Liquids Thiazolium Halogenide

2011 ◽  
Vol 332-334 ◽  
pp. 2036-2039 ◽  
Author(s):  
Qing Kai Wang ◽  
Hong Jun Zang ◽  
Fang Yang ◽  
Bo Wen Cheng ◽  
Yuan Lin Ren ◽  
...  
Keyword(s):  
Ionic Liquids ◽  
1H Nmr ◽  
Elemental Analysis ◽  
Room Temperature ◽  
High Conductivity ◽  
Room Temperature Ionic Liquids ◽  
Melting Points ◽  
Polar Solvents ◽  
Good Solubility

A series of novel thiazolium halogenide ionic liquids were synthesized by using 4-methylthiazole or 4-methyl-5-thiazoleethanol and halohydrocarbons as materials. The compounds were characterized and analyzed by elemental analysis, 1H NMR and DSC.The solubilities of the ionic liquids in organic dissolvents were observed, meanwhile the conductivities and melting points were measured. The results show that these ionic liquids have high conductivity in water and have good solubility in traditional polar solvents, such as H2O, ethanol and acetonitrile. And the thiazolium halogenide are room temperature ionic liquids, due to their low melting points.

scholarly journals Reactions of MoCl5 with 4-Methylpyridine, 2-Methylpyridine and 1-Methylimidazole in Tetrahydrofuran

2021 ◽  
Vol 37 (5) ◽  
pp. 1178-1186
Author(s):  
Rakesh Kumar ◽  
Gursharan Singh
Keyword(s):  
1H Nmr ◽  
13C Nmr ◽  
Room Temperature ◽  
Nitrogen Atmosphere ◽  
Transmission Mode ◽  
Vacuum Line ◽  
Ir Transmission ◽  
Ft Ir ◽  
Stoichiometric Ratios

MoCl5 reactions with 4-methylpyridine/2-methylpyridine/1-methylimidazole in THF in 1:1/1:2 stoichiometric ratios, at room temperature were carried out. The following products were synthesized: MoO2Cl(C6H7N), 1;Mo2O2Cl5(C6H7N)2(C4H8O)2,2; Mo4O4Cl4(C6H7N)3(C4H8O)2, 3 and Mo2O4Cl4(C4H6N)2(C4H8O), 4. These compounds have been investigated by FT-IR (transmission mode), FT-1H NMR, FT -13C NMR, microbiological, LC-MS and elemental (C, H, N, Mo, Cl) studies. In view of the sensitivity of all the reactants and products towards oxidation/hydrolysis by air/moisture, all the reactions and products were handled using dry nitrogen atmosphere in vacuum line. LC-MS and elemental studies agree with the formulae of compounds.

scholarly journals SYNTHESIS AND CONFORMATIONS OF p-(ACETAMIDO)-BUTOXYCALIX[4]ARENE AND p-(BENZAMIDO)-BUTOXYCALIX[4]ARENE

2010 ◽  
Vol 7 (2) ◽  
pp. 166-171
Author(s):  
Firdaus Firdaus ◽  
Jumina Jumina ◽  
Hardjono Sastrohamidjojo
Keyword(s):  
1H Nmr ◽  
Benzoyl Chloride ◽  
Room Temperature ◽  
Acetyl Chloride ◽  
13C Nmr Spectroscopy ◽  
Inert Atmosphere ◽  
Cone Conformation ◽  
Partial Cone ◽  
Temperature Method ◽  
Spectral Patterns

The conversion of p-(amino)butoxycalix[4]arene, 1, to p-(acetamido)butoxy-calix[4]arene, 2, and p-(benzamido)butoxycalix[4]arene, 3, via acetylation and benzoylation reactions, respectively have been conducted. The acetylation reactions was conducted by reflux method and room temperature method. The reflux method was conducted by refluxed a solution of 1 and acetic anhydride in acetic acid glacial solvent for 12 hours to result 2 in 53.8% yield; while the room temperature method was conducted by stirred a solution of 1, acetyl chloride, and dry pyridine in dry toluene solvent and inert atmosphere at room temperature for 24 hours to result 2 in 97.8% yield. By the room temperature method and using benzoyl chloride, the compound 3 was obtained in 67.1% yield. Structures of the both compounds were confirmed using IR, 1H NMR, and 13C NMR spectroscopy methods. Pursuant to the 1H-NMR spectral patterns of their bridge methylene and calix aryl protons, they were known that the compound 3 exist in partial cone conformation; whereas the compound 2 exist in partial cone, cone, and 1,2-alternate conformations where the partial cone was the main conformer.   Keywords: p-(amino)butoxycalix[4]arene, p-(acetamido)butoxycalix[4]arene, p-(benzamido)butoxycalix[4]arene,

Synthesis, Characterization, and Acid - Base Properties of Ruthenium(II) Complexes Containing N-ethyl-4-([1,10]-phenanthroline[5,6 - f]imidazol-2-yl)carbazole

2010 ◽  
Vol 63 (4) ◽  
pp. 700 ◽  
Author(s):  
Li Xu ◽  
Peng-Xin Liu ◽  
Guo-Liang Liao ◽  
Xiang Chen ◽  
Hui Chao ◽  
...  
Keyword(s):  
Cyclic Voltammetry ◽  
Nmr Spectroscopy ◽  
1H Nmr ◽  
Elemental Analysis ◽  
1H Nmr Spectroscopy ◽  
Room Temperature ◽  
Emission Spectra ◽  
Ph Effects ◽  
Acid Base ◽  
Polypyridyl Complexes

Three new ruthenium(ii) polypyridyl complexes, [Ru(phen)2(Hecip)]2+ (1), [Ru(phen)(Hecip)2]2+ (2), and [Ru(Hecip)3]2+ (3) complexes (phen = 1,10-phenanthroline, Hecip = N-ethyl-4-([1,10]-phenanthroline[5,6–f]imidazol-2-yl)carbazole) were synthesized and characterized by ES-MS, 1H NMR spectroscopy, elemental analysis, and cyclic voltammetry. The emission spectra of complexes were measured both at room temperature and at 77 K in a 4/1 (v/v) EtOH/MeOH matrix. All three complexes display luminescence properties which are close to that featured by the parent [Ru(phen)3]2+ species. The pH effects on the UV-vis and emission spectra of RuII complexes were also studied, and complexes 1, 2, and 3 were found to act as ‘on–off’ luminescent pH switches with maximum on–off ratios of 17, 230, and 90, respectively.

A Liquid Nitrogen Cooled Stage for STEM

1974 ◽  
Vol 32 ◽  
pp. 444-445
Author(s):  
Louis T. Germinario
Keyword(s):  
Electron Microscope ◽  
High Resolution ◽  
Liquid Nitrogen ◽  
Room Temperature ◽  
Objective Lens ◽  
Thermal Drift ◽  
Specimen Holder ◽  
Resolution Capability ◽  
Focal Position

A liquid nitrogen stage has been developed for the JEOL JEM-100B electron microscope equipped with a scanning attachment. The design is a modification of the standard JEM-100B SEM specimen holder with specimen cooling to any temperatures In the range ~ 55°K to room temperature. Since the specimen plane is maintained at the ‘high resolution’ focal position of the objective lens and ‘bumping’ and thermal drift la minimized by supercooling the liquid nitrogen, the high resolution capability of the microscope is maintained (Fig.4).

Synthesis, Characterization and Thermal studies of Novel Organomercury Driven from Sulfa Drugs Part 1

2011 ◽  
Vol 7 (2) ◽  
pp. 1338-1347
Author(s):  
Tarek Ali Fahad ◽  
Shaker.A.N. AL-Jadaan
Keyword(s):  
Thermal Decomposition ◽  
Thermal Behavior ◽  
1H Nmr ◽  
Elemental Analysis ◽  
Thermal Studies ◽  
Spectroscopic Techniques ◽  
Sulfa Drugs ◽  
Acid Base ◽  
Ph Values ◽  
Multi Stage

Two new heterocyclic Organmercury compounds   were prepared from the reaction of Sulfamethaxazole and Sulfadiazine with 4-acetaminophenol as a coupler and separated as solids with characteristic colors. these compounds were characterized by F.T.IR-spectroscopy 1H-NMR , Micro-elemental Analysis and UV-Vis spectroscopic techniques . The work involves a study of acid – base properties compounds at different pH values, the ionization and protonation constants were calculated. The thermal behavior of these two compounds   were investigated on the basis of thermogravimetric (TGA) and differential thermogravimetric (DTG) analyses, Thermal decomposition of these compounds is multi-stage processes.

Green synthesis of mixed metallic nanoparticles using room temperature self-assembly

2017 ◽  
Vol 13 (2) ◽  
pp. 4671-4677 ◽  
Author(s):  
A. M. Abdelghany ◽  
A.H. Oraby ◽  
Awatif A Hindi ◽  
Doaa M El-Nagar ◽  
Fathia S Alhakami
Keyword(s):  
Self Assembly ◽  
Metallic Nanoparticles ◽  
Room Temperature ◽  
Bimetallic Nanoparticles ◽  
Reduction Process ◽  
Nano Particles ◽  
Nano Structure ◽  
Small Shift ◽  
Molar Ratios ◽  
Vis Spectroscopy

Bimetallic nanoparticles of silver (Ag) and gold (Au) were synthesized at room temperature using Curcumin. Reduction process of silver and gold ions with different molar ratios leads to production of different nanostructures including alloys and core-shells. Produced nanoparticles were characterized simultaneously with FTIR, UV/vis. spectroscopy, transmission electron microscopy (TEM), and Energy-dispersive X-ray (EDAX). UV/vis. optical absorption spectra of as synthesized nanoparticles reveals presence of surface palsmon resonance (SPR) of both silver at (425 nm) and gold at (540 nm) with small shift and broadness of gold band after mixing with resucing and capping agent in natural extract which suggest presence of bimetallic nano structure (Au/Ag). FTIR and EDAX data approve the presence of bimetallic nano structure combined with curcumin extract. TEM micrographs shows that silver and gold can be synthesized separately in the form of nano particles using curcumin extract. Synthesis of gold nano particles in presence of silver effectively enhance and control formation of bi-metallic structure.

Synthesis and Biological Evaluation of Various New Substituted 1,3,4-oxadiazole-2-thiols

2008 ◽  
Vol 59 (4) ◽  
Author(s):  
Gabriela Laura Almajan ◽  
Stefania Felicia Barbuceanu ◽  
Ioana Saramet ◽  
Mihaela Dinu ◽  
Cristian Vasile Doicin ◽  
...  
Keyword(s):  
Biological Activity ◽  
Plant Growth ◽  
1H Nmr ◽  
Elemental Analysis ◽  
13C Nmr ◽  
Biological Evaluation ◽  
Ethyl Chloroacetate ◽  
Low Concentrations ◽  
Synthesis And Biological Evaluation

5-[4-(4X-phenylsulfonyl)phenyl]-1,3,4-oxadiazole-2-thiols, X=H, Cl, Br, reacted with ethyl chloroacetate to give S-alkylated compounds. Aminomethylation of the thione form of oxadiazoles yielded N(3)-derivatives. All the products have been characterized by elemental analysis, IR, 1H-NMR and 13C-NMR. The plant-growth regulating effects of the title compounds were examined. From the biological activity results, we found that most compounds showed weak stimulatory activities at low concentrations.

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