scholarly journals Design, synthesis and spectroscopic properties of crown ether-capped dibenzotetraaza[14]annulenes

2019 ◽  
Vol 15 ◽  
pp. 617-622 ◽  
Author(s):  
Krzysztof Miroslaw Zwoliński ◽  
Julita Eilmes
Keyword(s):  
Nmr Spectroscopy ◽  
Crown Ether ◽  
Elemental Analysis ◽  
Binding Sites ◽  
Spectroscopic Properties ◽  
Design Synthesis ◽  
Face To Face ◽  
C Nmr

The first crown ether-capped dibenzotetraaza[14]annulenes (DBTAAs), featuring two macrocyclic binding sites fixed in a face-to-face orientation, were synthesized in satisfactory 26–28% isolated yields. Direct N-alkylation of 1,4,10-trioxa-7,13-diazacyclopentadecane by symmetric DBTAA derivatives bearing bromoalkoxy pendants proceed smoothly at a reasonable level of dilution (1.25 mM). The structures were fully characterized by HR-ESIMS, FTIR-ATR, 1H and 13C NMR spectroscopy and elemental analysis.

Design, synthesis and crystallographic study of novel indole-based cyano derivatives as key building blocks for heteropolycyclic compounds of major complexity

2017 ◽  
Vol 73 (12) ◽  
pp. 1040-1049 ◽  
Author(s):  
Andrés C. García ◽  
Rodrigo Abonía ◽  
Luz M. Jaramillo-Gómez ◽  
Justo Cobo ◽  
Christopher Glidewell
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Ambient Temperature ◽  
Elemental Analysis ◽  
Building Blocks ◽  
Reaction Sequence ◽  
Design Synthesis ◽  
Crystallographic Study ◽  
Triclinic Form ◽  
C Nmr

A four-stage reaction sequence has been designed and developed for the synthesis of highly functionalized enolate esters as key building blocks for the synthesis of novel heteropolycyclic compounds of potential pharmaceutical value. The sequence starts with simple commercially available indoles and proceeds via 3-(indol-3-yl)-3-oxopropanenitriles, which react with 2-bromobenzaldehyde to form the corresponding chalcones; these are readily reduced to dihydrochalcones, which are in turn acylated to form the enolate esters. The compounds in this sequence have been characterized by IR and 1H and 13C NMR spectroscopy, by mass spectrometry and by elemental analysis. The molecular and supramolecular structures are reported for representative examples, namely (E)-3-(2-bromophenyl)-2-(1-methyl-1H-indole-3-carbonyl)acrylonitrile, C19H13BrN2O, (Ib), (2RS)-2-(2-bromobenzyl)-3-(1-methyl-1H-indol-3-yl)-3-oxopropanenitrile, C19H15BrN2O, (IIb), and (2RS)-3-(1-benzyl-1H-indol-3-yl)-2-(2-bromobenzyl)-3-oxopropanenitrile, C25H19BrN2O, (IIc), the latter two of which crystallize with Z′ = 2, and (E)-1-(1-acetyl-1H-indol-3-yl)-3-(2-bromophenyl)-2-cyanoprop-1-en-1-yl acetate, C22H17BrN2O, (III), and (E)-1-(1-benzyl-1H-indol-3-yl)-3-(2-bromophenyl)-2-cyanoprop-1-en-1-yl benzoate, C32H23BrN2O, (IV). The structure of the related chalcone (E)-2-benzoyl-3-(2-bromophenyl)prop-2-enenitrile, (V), has been redetermined at 100 K, where it is monoclinic, as opposed to the triclinic form reported at ambient temperature.

[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.

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

scholarly journals Synthesis and Single Crystal X-Ray Structure of Bis[4-oxo-3- (2-ethoxycarbonylphenyl)-3,4-dihydroquinazolin-2-yl]disulfide

2009 ◽  
Vol 64 (9) ◽  
pp. 1065-1069 ◽  
Author(s):  
Mehdi Rimaz ◽  
Jabbar Khalafy ◽  
Khadijeh Tavana ◽  
Katarzyna Ślepokura ◽  
Tadeusz Lis ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Structure Determination ◽  
Room Temperature ◽  
Sodium Ethoxide ◽  
Reaction Conditions ◽  
X Ray ◽  
Ethyl Nitroacetate ◽  
C Nmr

Diethyl 2,2´-thiocarbonyl-bis(azanediyl)dibenzoate was synthesized from the reaction of ethyl anthranilate with thiophosgene. Its treatment with sodium ethoxide in ethanol at room temperature gave ethyl 2-(4-oxo-2-thioxo-1,2-dihydroquinazolin-3(4H)-yl) benzoate, whereas in the presence of ethyl nitroacetate and under the same reaction conditions, the corresponding bis(quinazolin)disulfide was formed. Its structure was confirmed by IR, 1H and 13C NMR spectroscopy elemental analysis and single crystal X-ray structure determination.

scholarly journals Synthesis of cis, cis-1,3,5-trisubstituted cyclohexane based chelators with polyfunctional pendant arms

2005 ◽  
Vol 2005 (1) ◽  
pp. 43-45 ◽  
Author(s):  
Minati Baral ◽  
B.K. Kanungo ◽  
Peter Moore
Keyword(s):  
Schiff Base ◽  
Nmr Spectroscopy ◽  
Organic Compounds ◽  
Elemental Analysis ◽  
H Nmr ◽  
Benzenetricarboxylic Acid ◽  
New Compounds ◽  
Pendant Arms ◽  
C Nmr

Some novel organic compounds of the type: cis, cis-1,3,5-tris(X)cyclohexane, where X= –CONH(CH2)2NH2, –CONH(CH2)3NH2, –CONH(CH2)2NCH –C6H4OH, CONH(CH2)3NCHC6H4OH, which are expected to function as potential polydentate chelators have been synthesised from 1,3,5-benzenetricarboxylic acid through multi-steps reactions. 1,3,5-benzenetricarboxylic acid was reduced to cis, cis-1,3,5-tris(ethylcarboxylate)cyclohexane, which on reaction with excess of 1,2-diaminoethane and 1,2-diaminopropane afforded two new compounds. Condensation of the obtained derivatives with three equivalents of salicylaldehyde resulted the formation of two new Schiff base compounds. All the compounds were characterised by a combination of elemental analysis, mass, IR, UV-Vis, 1H NMR and 13C NMR spectroscopy.

scholarly journals Synthesis and Photophysical and Electrochemical Properties of Functionalized Mono-, Bis-, and Trisanthracenyl Bridged Ru(II) Bis(2,2′:6′,2″-terpyridine) Charge Transfer Complexes

2014 ◽  
Vol 2014 ◽  
pp. 1-10
Author(s):  
Adewale O. Adeloye ◽  
Peter A. Ajibade
Keyword(s):  
Charge Transfer ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Electrochemical Techniques ◽  
Visible Region ◽  
Charge Transfer Complexes ◽  
Cyclic Voltammograms ◽  
Butenoic Acid ◽  
Ft Ir ◽  
C Nmr

With the aim of developing new molecular devices having long-range electron transfer in artificial systems and as photosensitizers, a series of homoleptic ruthenium(II) bisterpyridine complexes bearing one to three anthracenyl units sandwiched between terpyridine and 2-methyl-2-butenoic acid group are synthesized and characterized. The complexes formulated as bis-4′-(9-monoanthracenyl-10-(2-methyl-2-butenoic acid) terpyridyl) ruthenium(II) bis(hexafluorophosphate) (RBT1), bis-4′-(9-dianthracenyl-10-(2-methyl-2-butenoic acid) terpyridyl) ruthenium(II) bis(hexafluorophosphate) (RBT2), and bis-4′-(9-trianthracenyl-10-(2-methyl-2-butenoic acid) terpyridyl) ruthenium(II) bis(hexafluorophosphate) (RBT3) were characterized by elemental analysis, FT-IR, UV-Vis, photoluminescence,1H and13C NMR spectroscopy, and electrochemical techniques by elemental analysis, FT-IR, UV-Vis, photoluminescence,1H and13C NMR spectroscopy, and electrochemical techniques. The cyclic voltammograms (CVs) of (RBT1), (RBT2), and (RBT3) display reversible one-electron oxidation processes atE1/2= 1.13 V, 0.71 V, and 0.99 V, respectively (versus Ag/AgCl). Based on a general linear correlation between increase in the length ofπ-conjugation bond and the molar extinction coefficients, the Ru(II) bisterpyridyl complexes show characteristic broad and intense metal-to-ligand charge transfer (MLCT) band absorption transitions between 480–600 nm,ε=9.45×103 M−1 cm−1, and appreciable photoluminescence spanning the visible region.

SYNTHESIS AND STUDY OF THE NEMATOCIDAL ACTIVITY OF 1,2,4-TRIAZOLO-1,2,4-TRIAZOLES

2020 ◽  
Vol 54 (1 (251)) ◽  
pp. 3-11
Author(s):  
M.A. Samvelyan ◽  
T.V. Ghochikyan ◽  
T.H. Yeganyan ◽  
M. Sarfraz ◽  
C. Jakob
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Thioglycolic Acid ◽  
Ethyl Esters ◽  
Steinernema Feltiae ◽  
Acid Basis ◽  
Biological Studies ◽  
Nematocidal Activity ◽  
C Nmr

The method has been developed for the preparation of ethyl esters of triazolo-substituted thioglycolic acid, basis on which the corresponding hydrazides, thiosemicarbazides and 1,2,4-triazolo-1,2,4-triazoles were synthesized by successive transformations. By the data of $ ^{1} \mathrm{H} $ and $ ^{13} \mathrm{C} $ NMR spectroscopy and elemental analysis have been established the structures of obtained compounds. Biological studies have shown that triazolo-triazoles at concentrations of 50 and 100 $ \mu m/mL $ reduce the viability of nematodes Steinernema Feltiae by 10–40%.

Nucleoside analogs involving modifications in the carbohydrate ring: nuclear magnetic resonance spectroscopic studies

1985 ◽  
Vol 63 (8) ◽  
pp. 2162-2168 ◽  
Author(s):  
Walter A. Szarek ◽  
B. Mario Pinto ◽  
Masaharu Iwakawa
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Nmr Spectroscopy ◽  
Magnetic Resonance ◽  
Nucleoside Analogs ◽  
Spectroscopic Properties ◽  
Spectroscopic Studies ◽  
Nucleoside Analog ◽  
H Nmr ◽  
Acyclic Nucleoside ◽  
C Nmr

The concomitant use of 1H nmr and 13C nmr spectroscopy as a probe of structure, stereochemistry, and conformation of several nucleoside analogs derived from 1-oxa-4-thiacyclohexane is described. The 1H nmr spectroscopic properties of an acyclic nucleoside analog derived from uridine are also described.

The first synthesis and characterization of new metal-free and metallophthalocyanine containing 33-membered crown ether moieties

2013 ◽  
Vol 17 (06n07) ◽  
pp. 473-479 ◽  
Author(s):  
Fatma Akkuş ◽  
Nilgün Kabay ◽  
Yaşar Gök
Keyword(s):  
Crown Ether ◽  
Spectral Data ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
The Novel ◽  
Metal Free ◽  
C Nmr

The synthesis and characterization of novel metal-free and metallophthalocyanines, fused symmetrically in non-peripheral positions with four octaoxamacrocycle has been synthesized by cyclotetramerization of the 2,5,8,11,14,20,23,26,29,32-decaoxatricyclo [31.2.2.115,19]octatriconta-1(36),15,17,19(38),33(37),34-hexaene-34,35-dicarbonitrile (5) which was prepared by the reaction of 3,6-bis[2-(2-{2-[2-(toluene-4-sulphonyl)-ethoxy]-ethoxy}-ethoxy)-ethoxy]-phthalonitrile (3) and 1,3-dihydroxybenzene (4). The novel compounds were characterized by using elemental analysis, 1 H , 13 C NMR, IR, UV-vis and MS spectral data.

Antiproliferative, antioxidant, computational and electrochemical studies of new azo-containing Schiff base ruthenium(ii) complexes

2018 ◽  
Vol 42 (4) ◽  
pp. 2952-2963 ◽  
Author(s):  
Ayşe İnan ◽  
Mesut İkiz ◽  
Seçil Erden Tayhan ◽  
Sema Bilgin ◽  
Nusret Genç ◽  
...  
Keyword(s):  
Schiff Base ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Electrochemical Studies ◽  
Uv Visible ◽  
C Nmr

A new series of ruthenium(ii) complexes 7–11 containing the –NN– group are synthesized and characterized via elemental analysis, and IR, UV-visible and 1H–13C NMR spectroscopy.

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