scholarly journals Synthesis of 4-[(1H-Benzimidazol-2-yl)sulfanyl]benzaldehyde and 2-({4-[(1H-Benzimidazol-2-yl)sulfanyl]phenyl}methylidene)hydrazine-1-carbothioamide

Molbank ◽  
10.3390/m1273 ◽  
2021 ◽  
Vol 2021 (3) ◽  
pp. M1273
Author(s):  
Mustafa Turki Ubeid ◽  
Hamdy Khamees Thabet ◽  
Mohamed Yousef Abu Shuheil
Keyword(s):  
Mass Spectrometry ◽  
Infrared Spectroscopy ◽  
Nmr Spectroscopy ◽  
High Yield ◽  
Reflux Temperature

Here we describe the preparation of 2-(4-((1H-benzo[d]imidazol-2-yl)thio)-benzylidene)-hydrazine-1-carbothioamide in two steps. In the first step, 1,3-dihydro-2H-1,3-benzimidazole-2-thione was reacted with 4-fluorobenzaldehyde in DMSO to get 4-[(1H-benzimidazol-2-yl)sulfanyl]benzaldehyde in high yield. The reaction of the obtained aldehyde with thiosemicarbazide in ethanol at reflux temperature yielded 2-({4-[(1H-benzimidazol-2-yl)sulfanyl]phenyl}methylidene)hydrazine-1-carbothioamide. The structure of the synthesized compounds was established by NMR spectroscopy (1H, 13C), mass spectrometry, and infrared spectroscopy.

scholarly journals Synthesis and reactions of alkenyl-gem-dichlorocyclopropanes obtained from piperylene

2020 ◽  
Vol 15 (5) ◽  
pp. 16-25
Author(s):  
A. I. Musin ◽  
Yu. G. Borisova ◽  
G. Z. Raskil’dina ◽  
R. U. Rabaev ◽  
R. R. Daminev ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Nmr Spectroscopy ◽  
High Yield ◽  
Quantitative Composition ◽  
Gas Liquid Chromatography ◽  
Liquid Chromatography Mass Spectrometry ◽  
Qualitative And Quantitative ◽  
Hardware Complex ◽  
Complex Mass

Objectives. This study aims to obtain alkenyl-gem-dichlorocyclopropanes from piperylene. The products are then subjected to thermocatalytic isomerization and hydrogenation.Methods. To determine the qualitative and quantitative composition of the reaction crudes, the following analytical methods were used: gas-liquid chromatography using the Crystal 2000 hardware complex, mass spectrometry using a Chromatec-Crystal 5000M device with the NIST 2012 database, and nuclear magnetic resonance (NMR) spectroscopy using a Bruker AM-500 device at operating frequencies of 500 and 125 MHz.Results. Alkenyl-gem-dichlorocyclopropanes were synthesized in the presence of triethylbenzyl ammonium chloride as catalyst. Their isomerization and hydrogenation gave the corresponding gem-dichlorocyclopentene and isomers of alkyl-gem-dichlorocyclopropanes. The structure of synthesized substances were analyzed by gas-liquid chromatography, mass spectrometry, and NMR spectroscopy.Conclusions. The results show that formation of four isomeric substituted gemdichlorocyclopropanes occurs in high yield during incomplete dichlorocyclopropanation of piperylene. The thermocatalytic isomerization of substituted gem-dichlorocyclopropanes in the presence of SAPO-34 zeolite leads to the formation of one product, i.e., gem-dichlorocyclopentene, and hydrogenation of substituted gem-dichlorocyclopropanes in the presence of Pd/C catalyst gives three isomeric alkyl-gem-dichlorocyclopropanes.

scholarly journals Different Coordination Modes of a Tripod Phosphine in Gold(I) and Silver(I) Complexes

1999 ◽  
Vol 6 (4-5) ◽  
pp. 211-221 ◽  
Author(s):  
P. Sevillano ◽  
M. E. García ◽  
A. Habtemariam ◽  
S. Parsons ◽  
P. J. Sadler
Keyword(s):  
Mass Spectrometry ◽  
Infrared Spectroscopy ◽  
Nmr Spectroscopy ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Fab Mass Spectrometry ◽  
Intramolecular Distance ◽  
Spectroscopy Studies ◽  
Linear Coordination

The following gold(I) and silver(I) complexes of the tritertiary phosphine 1,1,1- tris(diphenylphosphinomethyl)ethane, tripod , have been synthesised: Au3(tripod)X3 [X = Cl(1), Br(2), I(3)]; [Au3  (tripod)2Cl2  ]Cl (4); Au(tripod)X [X = Br(5), I(6)]; Ag3(tripod)(NO3)3 (7), Ag(tripod)NO3 (8). They were characterized by X-ray diffraction (complexes 2, 3 and 4), P31 NMR spectroscopy, electrospray and FAB mass spectrometry and infrared spectroscopy. Complexes 2 and 3 show a linear coordination geometry for Au(I), with relatively short Au-P bond distances. Complex 3 has a Au•••Au intramolecular distance of 3.326 A° , while complex 2 had a short Au•••Au intermolecular interaction of 3.048 A° . Complexes 4-6 were found by P31 NMR spectroscopy studies to contain a mixture of species in solution, one of which crystallised as [Au3(tripod|)2Cl2]Cl which was shown by X-ray diffraction to contain both tetrahedral and linear Au(I), the first example of a Au(I) complex containing such a mixture of geometries. The reaction of [Au3(tripod)Cl3] (1) with tripod led successfully to the formation of [Au3(tripod)Cl3][Au3(tripod|)2Cl2]+ and [Au3(tripod|)3Cl]2+ . The silver(I) complexes, 7 and 8 appear to contain linear and tetrahedral Ag(I), respectively.

scholarly journals Synthesis And Single Crystal X-Ray Structure Of 2-(1,3,4-Oxadiazol- 2-yl)Aniline

2007 ◽  
Vol 62 (6) ◽  
pp. 835-840 ◽  
Author(s):  
Ali Souldozi ◽  
Katarzyna Ślepokura ◽  
Tadeusz Lis ◽  
Ali Ramazani
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Single Crystal ◽  
Structure Determination ◽  
High Yield ◽  
Aminobenzoic Acid ◽  
Aromatic Rings ◽  
X Ray ◽  
C Nmr

Reaction of 2-aminobenzoic acid with (N-isocyanimino)triphenylphosphorane proceeds smoothly at r. t. to afford 2-(1,3,4-oxadiazol-2-yl)aniline in high yield. The structure of this compound was confirmed by IR, 1H, and 13C NMR spectroscopy, mass spectrometry, and single crystal X-ray structure determination. The X-ray structural analysis of the product indicated that its aromatic rings are approximately co-planar

Synthesis and studies of electrochemical properties of lophine derivatives

RSC Advances ◽  
2014 ◽  
Vol 4 (97) ◽  
pp. 54740-54746 ◽  
Author(s):  
A. Hariharasubramanian ◽  
Y. Dominic Ravichandran
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Fourier Transform ◽  
Liquid Chromatography ◽  
Infrared Spectroscopy ◽  
Nmr Spectroscopy ◽  
Magnetic Resonance ◽  
Electrochemical Properties ◽  
Fourier Transform Infrared Spectroscopy ◽  
Liquid Chromatography Mass Spectrometry

A versatile series of lophine derivatives (1–13) were synthesized and characterized, Fourier transform infrared spectroscopy (FTIR), Liquid Chromatography-Mass Spectrometry (LC-MS), and 1H and 13C nuclear magnetic resonance (NMR) spectroscopy.

Syntheses and Characterization of 1-Haloazagermatranes

2001 ◽  
Vol 56 (2) ◽  
pp. 137-140 ◽  
Author(s):  
Pavel L. Shutov ◽  
Sergey S. Karlov ◽  
Jörg Lorberth ◽  
Galina S. Zaitseva
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Molecular Composition ◽  
High Yield ◽  
Elemental Analyses ◽  
New Compounds ◽  
C Nmr

Abstract Germanium, Azagermatranes The reaction of tris(dimethylamino)halogermanes, (Me2N)3GeHal (7, Hal = Cl; 8 , Hal = Br), with tris(2-aminoethyl)amines, N(CH2CH2NHR)3 (5, R = H; 6 , R = Me), yield l-halo-N,N',N"-azagermatranes (1, X = Cl, R = H; 2, X = Br, R = H; 3, X = Cl, R = Me; 4, X = Br, R = Me). Treatment of 4 with n-butyllithium affords l-n-butyl-N,N',N"-trimethylazagermatrane (14) in high yield. Reactions of n-BuLi with 7 or (Me2N)4Ge (13) lead to the formation of (Me2N)3Ge-n-Bu (15). On treatment of 15 with 5 the 1 -n-butylazagermatrane 16 was obtained. The molecular composition and the structures of all new compounds were established by elemental analyses, 1H and 13C NMR spectroscopy and mass spectrometry.

scholarly journals Synthesis, characterization and DNA interaction studies of new triptycene derivatives

2014 ◽  
Vol 10 ◽  
pp. 1290-1298 ◽  
Author(s):  
Sourav Chakraborty ◽  
Snehasish Mondal ◽  
Rina Kumari ◽  
Sourav Bhowmick ◽  
Prolay Das ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Conformational Changes ◽  
Dna Interaction ◽  
High Yield ◽  
Efficient Synthesis ◽  
Elemental Analyses ◽  
Multinuclear Nmr Spectroscopy ◽  
Propiolic Acid

A facile and efficient synthesis of a new series of triptycene-based tripods is being reported. Using 2,6,14- or 2,7,14-triaminotriptycenes as synthons, the corresponding triazidotriptycenes were prepared in high yield. Additionally, we report the transformation of 2,6,14- or 2,7,14-triaminotriptycenes to the corresponding ethynyl-substituted triptycenes via their tribromo derivatives. Subsequently, derivatization of ethynyl-substituted triptycenes was studied to yield the respective propiolic acid and ethynylphosphine derivatives. Characterization of the newly functionalized triptycene derivatives and their regioisomers were carried out using FTIR and multinuclear NMR spectroscopy, mass spectrometry, and elemental analyses techniques. The study of the interaction of these trisubstituted triptycenes with various forms of DNA revealed interesting dependency on the functional groups of the triptycene core to initiate damage or conformational changes in DNA.

Synthesis and Caracterization of some New 1H-3-aryl-7-etoxycarbonyl-6-methyl-pyrazolo[5,1-c][1,2,4]triazoles

2008 ◽  
Vol 59 (1) ◽  
pp. 41-44
Author(s):  
Maria-Daniela Sofei ◽  
Maria Ilici ◽  
Valentin Badea ◽  
Carol Csunderlik ◽  
Vasile-Nicolae Bercean
Keyword(s):  
Mass Spectrometry ◽  
Acetic Acid ◽  
Nmr Spectroscopy ◽  
Sodium Acetate ◽  
Glacial Acetic Acid ◽  
Ir And Nmr Spectroscopy

The synthesis of 1H-3-aryl-7-ethoxycarbonyl-6-methyl-pyrazolo[5,1-c][1,2,4]triazoles (2) was carried out by cyclization of 1H-5-arylidenehydrazino-4-ethoxycarbonyl-3-methyl-pyrazoles (1) in the presence of bromine using glacial acetic acid as solvent and sodium acetate as base. The new nine obtained compounds were characterized by IR and NMR spectroscopy and mass spectrometry.

The mechanism of formation of 2,7-dimethyl-2,6-octadiene in the synthesis of 3-methylene-7-methyl-1,6-octadiene

1983 ◽  
Vol 48 (7) ◽  
pp. 1864-1866
Author(s):  
Jan Bartoň ◽  
Ivan Kmínek
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Alkali Metal ◽  
Chromatographic Analysis ◽  
Solid Phase ◽  
Reaction Pathway ◽  
Mechanism Of Formation ◽  
Gas Chromatographic Analysis ◽  
C Nmr ◽  
Visual Observations

2,7-Dimethyl-2,6-octadiene is formed in the catalytic solution for the dimerization of 2-methyl-1,3-butadiene to β-myrcene (3-methylene-7-methyl-1,6-octadiene), as revealed by mass spectrometry and 13C NMR spectroscopy. Visual observations together with the results of gas chromatographic analysis of the catalytic solution suggest that the formation of 2,7-dimethyl-2,6-octadiene is associated with the transition of the alkali metal (sodium) from the solid phase into the solution. A reaction pathway is suggested accounting for the formation of 2,7-dimethyl-2,6-octadiene in the system.

A New Dimeric Derivative of Ethoxyquin from Its Reaction with Alkylperoxy Radicals

1993 ◽  
Vol 58 (8) ◽  
pp. 1914-1918 ◽  
Author(s):  
Jaroslav Kříž ◽  
Luděk Taimr
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Peroxy Radicals ◽  
Methyl Group ◽  
Alkylperoxy Radicals ◽  
C Nmr

The structure of a new compound formed in the reaction of ethoxyquin with alkylperoxy radicals was resolved by 1H and 13C NMR spectroscopy (including COSY, NOESY, HHC RCT and SSLR INEPT techniques) and confirmed by mass spectrometry. The structure suggest participation of 4-methyl group of ethoxyquin in the deactivation of peroxy radicals. A mechanism of this reaction is proposed.

Ten-Vertex Polyhedral Monocarbaborane Chemistry. The Novel High-Yield Formation of the Ten-Vertex closo Compound [6-(PMe2Ph)-closo-1-CB9H9] from the Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11]

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
High Yield ◽  
Monoclinic Space Group ◽  
The Novel ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
X Ray ◽  
Yield Formation ◽  
Boiling Toluene

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.

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