Synthesis, Characterization and Complexation Studies with K + and Ca2+ Cations of trans-1.2-Cyclohexanedioxydiacetamides

1988 ◽  
Vol 43 (2) ◽  
pp. 165-170 ◽  
Author(s):  
Whei Oh Lin ◽  
Maria C. B. V. de Souza ◽  
Helmut G. Alt
Keyword(s):  
Nmr Spectroscopy ◽  
Mass Spectroscopy ◽  
H Nmr ◽  
Coordination Sites ◽  
Complexation Studies ◽  
Ir And Nmr Spectroscopy ◽  
Elemental Analyses ◽  
C Nmr

The synthesis of trans-1.2-cyclohexanedioxydiacetamides starting with trans-1.2-cyclohexane-diol is described. Eleven of these compounds are characterized by IR, 1H NMR, 13C NMR and mass spectroscopy as well as elemental analyses. Most of these compounds are suitable ionophors for the cations K+ and Ca2+. The coordination sites of these ligands in the 1:2 complexes were determined by IR and NMR spectroscopy

1,2-Bis(1-aryl-3-alkyltriazen-3-yl)ethanes and related compounds

1998 ◽  
Vol 76 (1) ◽  
pp. 125-135 ◽  
Author(s):  
Donald L Hooper ◽  
Ian R Pottie ◽  
Marc Vacheresse ◽  
Keith Vaughan
Keyword(s):  
Nmr Spectroscopy ◽  
Line Broadening ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Ir And Nmr Spectroscopy ◽  
Diazonium Coupling ◽  
Significant Line ◽  
Related Compounds ◽  
C Nmr

A series of novel bistriazenes, the 1,2-bis(1-aryl-3-methyltriazen-3-yl)ethanes, Ar-N T N-NMe-CH2CH2-NMe-N T N-Ar, have been synthesized by diazonium coupling with N,N'-dimethylethylenediamine. These bistriazenes are stable crystalline compounds and have been unequivocally characterized by IR and NMR spectroscopy (1H and 13C), and elemental analysis. The structures of two compounds in the series have been confirmed by X-ray crystallography. The 1H NMR spectra show significant line broadening of the N-methyl resonances arising from the restricted rotation around the N2-N3 bond of the triazene units. The presence of strongly electron-withdrawing groups on the aryl ring restricts the rotation to the point where the N-methyl signals of the rotamers are distinct even at room temperature; four resonances of the N-methyl signal are clearly evident and these can be assigned to the anti-anti, syn-syn, and syn-anti conformations of the bistriazene. Diazonium coupling with N,N'-diethylethylenediamine affords the N,N'-diethyl homologues of the bistriazenes, which have been similarly characterized. As model compounds to assist in spectroscopic analysis, a series of related triazenes, the 1-(1-aryl-3-methyltriazen-3-yl)-N,N-dimethyl-2-ethanamines, were prepared by diazonium coupling with N,N,N'-trimethylethylenediamine. These dialkyltriazenes exist mainly as oils, but characterization was achieved by IR, 1H NMR, and 13C NMR spectroscopy, also showing the presence of two rotamers in solution when strongly electron-withdrawing substituents are bonded to the aryl moiety.Key words: triazene, bistriazene, diazonium, ethylenediamine, molecular dynamics, NMR.

Übergangsmetall-Carbin-Komplexe, XC. Synthese neuer, siebenfach-koordinierter, kationischer Carbin-Komplexe des Wolframs in einer höheren Oxidationszahl / Transition Metal Carbyne Complexes, XC. Synthesis of New, Seven Coordinated, Cationic Tungsten Carbyne Complexes in a Higher Oxidation State

1988 ◽  
Vol 43 (6) ◽  
pp. 654-657 ◽  
Author(s):  
Alexander Constantin Filippou ◽  
Ernst Otto Fischer ◽  
Helmut Guido
Keyword(s):  
Electrical Conductivity ◽  
Nmr Spectroscopy ◽  
Transition Metal ◽  
Carbonyl Group ◽  
Oxidation State ◽  
Ionic Character ◽  
H Nmr ◽  
Elemental Analyses ◽  
Carbyne Complexes ◽  
C Nmr

The reaction of (I)3(CO)L2W≡CNEt2 (L2 = 2.2'-bipyridyl(2.2'-bipy); 1.10-phenanthroline (ophen)) (1, 2) with two equivalents of tert-butylisonitrile results in the elimination of the carbonyl group and the displacement of one iodine ligand from the coordination sphere, leading to the new, cationic carbyne complexes [(I)2(t-C4H9NC)2L2W≡CNEt2]+I- (3, 4). The ionic character and composition of 3 and 4 was confirmed by the electrical conductivity of their solutions as well as by elemental analyses, IR, 1H NMR and 13C NMR spectroscopy.

Dioxa-dithia Macrocycle-bridged Dimeric with Hexakis(alkylthio) Substituents and Network Polymer Phthalocyanines

1997 ◽  
Vol 01 (01) ◽  
pp. 67-76 ◽  
Author(s):  
A. G. GÜREK ◽  
Ö. BEKARO ĞLU
Keyword(s):  
Electrical Conductivity ◽  
Nmr Spectroscopy ◽  
Chemical Doping ◽  
The Novel ◽  
Conductivity Measurements ◽  
Network Polymer ◽  
Network Polymers ◽  
H Nmr ◽  
Elemental Analyses ◽  
C Nmr

1,7-dithia (12-crown-4)-bridged phthalocyanine network polymers were prepared from tetracyanodibenzo-[1,7-dithia(12-crown-4)]. In addition, the synthesis of two 1,7-dithia (12-crown-4) linked peripherally octa-substituted dimeric phthalocyanines, which contain a combination of hexakis(alkylthia) side chains, is described. These extremely soluble compounds were prepared by the condensation of an iminoisoindoline derivative and a subphthalocyanine. The novel compounds are characterized by elemental analyses, UV/vis, IR, mass, 1 H NMR and 13 C NMR spectroscopy. The electrical conductivity measurements of three of the four network polymers were unsuccessful; however chemical doping with NOBF 4 could be increased to a measurable value. The electrical conductivity of the dimeric phthalocyanines are in the semiconductor range.

Synthesis of 1,3-diazaspiro[5,5]undecanes and 1-thia-3-azaspiro[5,5]undec-2-enes by reaction of 2-cyanocyclohexylideneacetyl isothiocyanate with amines and sodium hydrogen sulfide

1987 ◽  
Vol 52 (4) ◽  
pp. 989-994 ◽  
Author(s):  
Milan Dzurilla ◽  
Ondrej Forgáč ◽  
Peter Kutschy ◽  
Pavol Kristian ◽  
Dušan Koščík ◽  
...  
Keyword(s):  
Hydrogen Sulfide ◽  
Alkaline Medium ◽  
Mass Spectroscopy ◽  
Aromatic Amines ◽  
Secondary Amines ◽  
H Nmr ◽  
Sodium Hydrogen ◽  
Elemental Analyses ◽  
Primary Aromatic Amines ◽  
C Nmr

2-Cyanocyclohexylideneacetyl isothiocyanate (II) reacts with sodium hydrogen sulfide to give 1-thia-3-azaspiro[5,5]undecane. Reaction of II with secondary amines afforded 1-thia-3-azaspiro[5,5]undec-2-enes whereas primary aromatic amines gave 1,3-diazaspiro[5,5]undecanes under the same conditions. Both types of reactions proceed via substituted thioureas which were isolated pure only in the case of 4-methylaniline and 4-methoxyaniline. They were cyclized in alkaline medium to the corresponding diazaspiro derivatives. The structure of the synthesized compounds was confirmed by their elemental analyses and IR, 1H NMR, 13C NMR and mass spectroscopy.

An Efficient Synthesis of 1-Thia-5-azaspiro[5.5]undec-2-ene and its Recyclization to 1,5-Diazaspiro[5.5]undec-2-ene and/or Spiro-Thieno[2,3-d]pyrimidin-4(1H)-one Derivatives

2011 ◽  
Vol 66 (5) ◽  
pp. 487-492
Author(s):  
Raafat M. Shaker ◽  
Asmaa Hamoda ◽  
Yusria R. Ibrahim ◽  
Kamal M. El-Shaieb ◽  
Fathy F. Abdel-Latif
Keyword(s):  
Nmr Spectroscopy ◽  
Direct Synthesis ◽  
Efficient Synthesis ◽  
H Nmr ◽  
Elemental Analyses ◽  
C Nmr

An efficient and direct synthesis of 1-thia-5-azaspiro[5.5]undec-2-ene is described, and the basecatalyzed recyclization of this compound was studied. The products have been characterized by elemental analyses, and IR, MS, 1H NMR, and 13C NMR spectroscopy

[Zn(phen)2(CX3COO)]+, X = H orCl; Influence of X on the Coordination Mode of the Carboxylate Group (phen = 1,10-Phenanthroline)

2005 ◽  
Vol 60 (10) ◽  
pp. 1049-1053 ◽  
Author(s):  
Zeanab Talaei ◽  
Ali Morsali ◽  
Ali R. Mahjoub
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Coordination Mode ◽  
Bidentate Ligand ◽  
Carboxylate Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Coordinate Geometry ◽  
C Nmr

Two new ZnII(phen)2 complexes with trichloroacetate and acetate anions, [Zn(phen)2(CCl3COO)- (H2O)](ClO4) and [Zn(phen)2(CH3COO)](ClO4), have been synthesized and characterized by elemental analysis, IR, 1H NMR, 13C NMR spectroscopy. The single crystal X-ray data of these compounds show the Zn atoms to have six-coordinate geometry. From IR spectra and X-ray crystallography it is established that the coordination of the COO− group is different for trichloroacetate and acetate. The former acts as a monodentate whereas the latter acts as a bidentate ligand.

scholarly journals Three-Dimensional Supramolecular Network Directed by Intermolecular Interactions in [Pb2(dmp)2(hfacac)4]

2009 ◽  
Vol 6 (4) ◽  
pp. 1085-1090
Author(s):  
Farzin Marandi ◽  
Lotfali Saghatforoush ◽  
Hossein Farzaneh
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Three Dimensional ◽  
Supramolecular Network ◽  
Stacking Interactions ◽  
H Nmr ◽  
Noncovalent Bond ◽  
Donor And Acceptor ◽  
Anionic Ligands ◽  
C Nmr

To investigate the interactions between noncovalent bond donor and acceptor giving rise to three dimensional networks, compound [Pb2(dmp)2(hfacac)2] (1) (dmp = 2,9-dimethyl-1,10-henanthroline and Hhfacac = hexafluoroacetylacetonate) has been prepared and characterized by elemental analysis, IR,1H NMR, and13C NMR spectroscopy and its crystal structures was investigated. The single crystal structure show the coordination number of Pb(II) to be eight with twoN-donor atoms from a “dmp” ligand and sixO-donors from the anionic ligands. The supramolecular structure of 1 is realized by weak directional C–H∙∙∙O–C, C–F∙∙∙F–C andπ–πstacking interactions.

scholarly journals Synthesis of Some Novel Fused Imidazo [2, 1-b] [1, 3] Thiazole and Imidazo [2, 1-b] Thiazolo [5, 4-d] Isoxazole Derivatives

2012 ◽  
Vol 9 (3) ◽  
pp. 1518-1525 ◽  
Author(s):  
Hamid Reza Jaberi ◽  
Hadi Noorizadeh
Keyword(s):  
Acetic Acid ◽  
Sodium Acetate ◽  
Carbon Disulphide ◽  
Thiazole Derivatives ◽  
H Nmr ◽  
Nmr Data ◽  
Elemental Analyses ◽  
New Compounds ◽  
Isoxazole Derivatives ◽  
C Nmr

In this work we describe the synthesis of some novel fused imidazo [2, 1-b] [1, 3] thiazole derivatives. The reaction of 1, 2-diaminoethane 1 with carbon disulphide in H2O/ETOH as solvent furnishes 4, 5-dihydro-1H-imidazol-2-thiol 2 under reflux condition. the reaction of 4,5-dihydro-1H-imidazol-2-thiol on treatment with ethylchloro acetate and aromatic aldehyde in presence of anhydrous sodium acetate and acetic acid as solvent to give (Z)-2-(arylidene)-5,6-dihydroimidazo [2,1-b] [1,3] thiazol-3(2H)-one 3a-j. Compounds 3a-j was condensed with hydroxylamine to give 3-(aryl)-2, 3, 6, 7-tetrahydroimidazo [2, 1-b] [1,3] thiazolo [5, 4-d] isoxazole 4a-j. The structures of the new compounds were established by elemental analyses, IR,1H NMR and13C NMR data.

Synthesen und Reaktionen von schwefelkoordinierten Ruthenium-Komplexen [1]/Syntheses and Reactions of Sulfur Coordinated Ruthenium Complexes [1]

1982 ◽  
Vol 37 (8) ◽  
pp. 1026-1033 ◽  
Author(s):  
Dieter Sellmann ◽  
Elmar Böhlen
Keyword(s):  
Mass Spectroscopy ◽  
Ruthenium Complexes ◽  
H Nmr ◽  
Elemental Analyses

Abstract The syntheses and reactions of sulfur coordinated ruthenium centers with CO, PR3, (R = Me, Ø), N2H4 and N2 are investigated. Reaction of [Ru(CO)3(THF)Cl2] with lithium-o-methylthiobenzenethiolate yields cis-[Ru(CO)2(CH3S-C6H4-S)2], with Li2-o-benzenedithiolate the cis-[Ru(CO)2(C6H4S2)2]2--ion is obtained, which can be isolated either as the NMe4 salt or reacted further with 1,2-C2H4Br2 to give cis-[Ru(CO)2dttd], (dttd2-= 2,3,8,9-Dibenzo-1,4,7,10-tetrathiadecane2-). In all three complexes the CO ligands are relatively inert to substitution; refluxing of [Ru(CO)2(C6H4S2)2]2- in EtOH in the presence of excess PMe3, however, and subsequent alkylation with 1,2-C2H4Br2 yields [Ru(CO)PMe3(dttd)]. [Ru(PMe3)2dttd] is obtained from [Ru(PMe3)4Cl2] and Li2-dttd, the synthesis of which is also described. In [Ru(PMe3)2(dttd)] the PMe3 ligands are inert, but in [Ru(PØ3)2(dttd)] one PØ3 ligand is easily substituted by CO or N2H4 yielding [Ru(CO)(PØ3)dttd] or [Ru(N2H4)(PØ3)dttd] respectively; [Ru(PØ3)2(dttd)] is obtained from [RU(PØ3)3Cl2] and H2-dttd. The complexes are characterized by elemental analyses, IR, 1H NMR and mass spectroscopy.

Synthesis and Pharmacological Activities of Some New 2-[1-Heptyl-3-(4- methoxybenzyl)-5-oxo-1,5-dihydro-4H-1,2,4-triazol-4-yl]acetohydrazide Derivatives

2014 ◽  
Vol 69 (9-10) ◽  
pp. 969-981 ◽  
Author(s):  
Olcay Bekircan ◽  
Emre Mentese ◽  
Serdar Ulker
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Lipase Activity ◽  
Spectral Studies ◽  
Antituberculosis Activity ◽  
Pharmacological Activities ◽  
Mass Spectral ◽  
H Nmr ◽  
Acetohydrazide Derivative ◽  
C Nmr

Abstract In the present investigation, the key intermediate acetohydrazide derivative 5 was synthesized starting from 3-(4-methoxybenzyl)-4-amino-4,5-dihydro-1,2,4-triazol-5-one (1) by a four-step reaction. Thiosemicarbazides 6a-f and arylidenehydrazide derivatives 8a-d were obtained from compound 5. The cyclization of compounds 6a-f in the presence of NaOH resulted in the formation of compounds 7a-f. The compounds were characterized by IR, 1H NMR, 13C NMR spectroscopy, elemental analysis and mass spectral studies. The compounds were tested for their anti-lipase, anti-α-glucosidase and anti-mycobacterial activities. Compounds 6b and 8c exhibited excellent anti-lipase activity, and compound 8d showed excellent anti-a-glucosidase activity. Compounds 3 and 4 exhibited good antituberculosis activity

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