scholarly journals Synthesis and Spectroscopic Characterization of Some New Axially Ligated Indium(III) Macrocyclic Complexes and Their Biological Activities

2014 ◽  
Vol 2014 ◽  
pp. 1-7
Author(s):  
Gauri D. Bajju ◽  
Altaf Ahmed ◽  
Deepmala Gupta ◽  
Ashu Kapahi ◽  
Gita Devi
Keyword(s):  
Biological Activities ◽  
Spectroscopic Characterization ◽  
Axial Ligand ◽  
Free Base ◽  
H Nmr ◽  
Pyramidal Geometry ◽  
The Stability ◽  
Square Pyramidal Geometry ◽  
C Nmr

The synthesis and spectroscopic characterization of new axially ligated indium(III) porphyrin complexes were reported. Chloroindium(III) porphyrin (TPPIn-Cl) was obtained in good yield by treating the corresponding free base with indium trichloride. The action of the different phenols on chloroderivatives (TPPIn-Cl) led to the corresponding phenolato complexes (TPPIn-X). These derivatives were characterized on the basis of mass spectrometry,1H-NMR, IR, and UV-visible data. The separation and isolation of these derivatives have been achieved through chromatography. The spectral properties of free base porphyrin and its corresponding metallated and axially ligated indium(III) porphyrin compounds were compared with each other. A detailed analysis of UV-Vis,1H-NMR, and IR suggested the transformation from free base porphyrin to indium(III) porphyrin. Besides,13C-NMR and fluorescence spectra were also reported and interpreted. The stability of these derivatives has also been studied through thermogravimetry. The complexes were also screened for anticancerous activities. Among all the complexes, 4-MePhO-InTPP shows highest anticancerous activity. The title complexe, TPPIn-X (where X = different phenolates), represents a five-coordinate indium(III) porphyrin complex in a square-pyramidal geometry with the phenolate anion as the axial ligand.

Synthesis and Characterization of a New Coumarin-1,2,3-Triazole Diad

2014 ◽  
Vol 618 ◽  
pp. 170-174
Author(s):  
Hong Qi Li ◽  
Xiu Juan Tian ◽  
Zhen Chen ◽  
Ding Xiao ◽  
Ning Fang ◽  
...  
Keyword(s):  
Click Chemistry ◽  
Biological Activities ◽  
Antitubercular Activity ◽  
Synthesis And Characterization ◽  
Target Compound ◽  
H Nmr ◽  
Mild Conditions ◽  
Ideal Approach ◽  
C Nmr

A new coumarin-1,2,3-triazole diad was designed and synthesized by Pechmann-Duisberg reaction and click chemistry. The three-step synthetic route to the target compound afforded an overall yield of 56%. The structures of the synthesized compounds were characterized by 1H NMR, 13C NMR, IR and mass spectrum. The click chemistry provided an ideal approach for synthesis under mild conditions of coumarin-1,2,3-triazole diads which may exhibit excellent biological activities such as antitubercular activity.

scholarly journals Synthesis and Spectroscopic Characterization of Some New Biological Active Azo–Pyrazoline Derivatives

2012 ◽  
Vol 9 (3) ◽  
pp. 1613-1622 ◽  
Author(s):  
Farouq E. Hawaiz ◽  
Mohammad K. Samad
Keyword(s):  
Addition Reaction ◽  
Coupling Reaction ◽  
Spectroscopic Characterization ◽  
Hydroxyl Group ◽  
Significant Activity ◽  
H Nmr ◽  
Ft Ir ◽  
High Yields ◽  
C Nmr

A number of 3-[4-(benzyloxy)-3-(2-Chlorophenylazo)-phenyl]-5-(substituted-phenyl)-1-substituted-2-pyrazolines( 4a-j) and (5a-j) have been synthesized by diazotization of 2-chloroaniline and its coupling reaction with 4-hydroxy acetophenone, followed by benzyloxation of the hydroxyl group to give the substrate [4-benzyloxy-3-(2-chlorophenylazo)-acetophenone (1)].The prepared starting material (1) has been reacted with different substituted benzaldehydes to give a new series of chalcone derivatives 1-[(4-benzyloxy)-3-(2-chloro-phenylazo)-phenyl]-3-(substituted phenyl)-2-propen-1-one (3a-j), in high yields and in a few minutes, and the later compounds were treated with hydrazine hydrate according to Michael addition reaction to afford a new biolological active target compounds (4a-j) and (5a-j). Furthermore, The structures of the newly synthesized compounds were confirmed by FT-IR,13C-NMR,13C-DEPT &1H-NMR spectral data. The chalcone and pyrazoline derivatives were evaluated for their anti bacterial activity againstEscherichia colias gram negative andStaphylococcus aureusas gram positive, the results showed significant activity against both types of bacteria.

scholarly journals Synthesis and Characterization of Novel 1,3-Thiazole and 2-Amino-1,3,4-Thiadiazole Derivatives

2014 ◽  
Vol 33 (2) ◽  
pp. 189 ◽  
Author(s):  
Mustafa Er ◽  
Ayşe Şahin ◽  
Hakan Tahtacı
Keyword(s):  
Biological Activities ◽  
High Yield ◽  
Synthesis And Characterization ◽  
Hantzsch Reaction ◽  
H Nmr ◽  
Thiadiazole Derivatives ◽  
High Yields ◽  
Mass Spectrometric Techniques ◽  
C Nmr

<p>Thiosemicarbazone derivatives <strong>3a–e</strong> were synthesized by the reaction of various aldehydes<strong> 1a–e</strong> with 4-methyl thiosemicarbazide <strong>2</strong> in 78% to 90% yield. Then, the thiazole moieties of the target materials <strong>5a–e</strong> were obtained in high yields (71–93%) using the Hantzsch reaction utilizing thiosemicarbazone derivatives <strong>3a–e</strong> with ethyl-2-chloroacetoacetic ester. The substituted nitrile derivatives <strong>7a–e</strong> were obtained in moderate to high yield (58–84%) from the reaction of compounds <strong>5a–e</strong> with chloroacetonitrile by the nucleophilic aliphatic substitution reaction in the presence of anhydrous potassium carbonate. Finally, substituted 2-amino-1,3,4-thiadiazole compounds <strong>9a–e</strong> were obtained in moderate to good yields (51–62%) from the reaction of thiosemicarbazide with substituted nitrile derivatives <strong>7a–e</strong>. As a result, compounds that all share a high disposition for biological activities were obtained. The structures of the newly synthesized compounds were confirmed by IR, <sup>1</sup>H NMR, <sup>13</sup>C NMR, elemental analysis, and mass spectrometric techniques.</p>

Chemistry of early and late transition metallaboranes: synthesis and structural characterization of periodinated dimolybdaborane [(Cp*Mo)2B4H3I5]

2015 ◽  
Vol 87 (2) ◽  
pp. 195-204 ◽  
Author(s):  
K. Yuvaraj ◽  
Dipak Kumar Roy ◽  
C. Arivazhagan ◽  
Bijnaneswar Mondal ◽  
Sundargopal Ghosh
Keyword(s):  
Solid State ◽  
Crystallographic Analysis ◽  
Late Transition Metals ◽  
Pyramidal Geometry ◽  
Late Transition ◽  
Solid State Structures ◽  
Square Pyramidal Geometry ◽  
C Nmr

AbstractThermolysis of an in situ generated intermediate [(Cp*Ta)2(BH3)2Cl2], 1 generated from the reaction of [Cp*TaCl4], (Cp* = η5-C5Me5) and [LiBH4·thf], in presence of [Ru3(CO)12] yielded pileo-[Cp*TaCl(μ-Cl)-B2H4Ru3(CO)8], 2 having two electrons fewer than seven pairs required for the observed square pyramidal geometry. Cluster 2 is the first example of an unsaturated cluster comprising early and late transition metals in a square pyramid core. This reaction also yielded [(Cp*Ta)2(B2H6)(B2H4Cl2)], 3 as a by-product. In addition, the reaction of [Cp*MoCl4] (Cp* = η5-C5Me5) with [LiBH4.thf] in presence of excess [MeI] at mild condition led to the isolation of periodinated dimolybdatetraborane [(Cp*Mo)2B4H3I5], 4 that hints a possible existence of [(Cp*Mo)2B4H8]. After the isolation of periodinated 4, we extended this chemistry towards the late transition metallaborane [(Cp*Rh)3B4H4], 5 using [PtBr2] as brominating source. Although all the attempts to isolate perbrominated rhodaborane failed, we have isolated partially brominated rhodaborane clusters [(Cp*Rh)3(BH)-(BBr)3], 6 and [(Cp*Rh)3(BH)3(BBr)], 7. All the compounds were characterized by IR and 1H, 11B and 13C NMR spectroscopy in solution, and the solid-state structures of 2, 4 and 6 were established by crystallographic analysis.

Formation and characterization of five- and six-coordinate iron(III) corrolazine complexes

2012 ◽  
Vol 16 (05n06) ◽  
pp. 518-529 ◽  
Author(s):  
Satoshi Kurahashi ◽  
Takahisa Ikeue ◽  
Tamotsu Sugimori ◽  
Masashi Takahashi ◽  
Masahiro Mikuriya ◽  
...  
Keyword(s):  
Ground State ◽  
Electronic Structures ◽  
Axial Ligand ◽  
Squid Magnetometry ◽  
Close Inspection ◽  
H Nmr ◽  
Axial Ligands ◽  
Excess Amount ◽  
C Nmr

Electronic structures of five- and six-coordinate iron(III) corrolazine complexes are determined by means of 1H NMR, 13C NMR, EPR, and Mössbauer spectroscopy as well as SQUID magnetometry. A series of five-coordinate complexes, [FeIII(TBP8Cz)(L)]* where the axial ligands(L) are cyanide(CN-), imidazole(HIm), 1-methylimidazole(1-MeIm), 4-(N,N-dimethylamino)pyridine(DMAP), pyridine(Py), 4-cyanopyridine(4-CNPy), and tert-butylisocyanide(tBuNC), are obtained by the addition of 1 to 2 equiv. of the ligands to the dichloromethane solutions of FeIII(TBP8Cz) at 298 K: TBP8Cz is a trianion of 2,3,7,8,12,13,17,18-octakis(4-tert-butylphenyl)corrolazine. These complexes commonly show the S = 3/2 at 298 K. By contrast, formation of the six-coordinate complexes depends on the nature of the axial ligands. While the addition of 3 equiv. of CN- has completely converted FeIII(TBP8Cz) to (Bu4N)2[FeIII(TBP8Cz)(CN)2] at 298 K, the conversion to the bis-adduct is only attained below ca. 200 K in the case of HIm, 1-MeIm, and DMAP even in the presence of 50 equiv. of the ligands. If the axial ligand is Py, 4-CNPy, or tBuNC, the formation of [FeIII(TBP8Cz)(L)2] is confirmed only at an extremely low temperature (15 K). Close inspection of the 1H NMR and EPR spectra has revealed that all the bis-adducts adopt the (dxy)2(dxz, dyz)3 ground state. While FeIII(TBP8Cz) forms paramagnetic bis- and mono-adduct in toluene solution at 298 K in the presence of excess amount of CN- and tBuNC, respectively, the corresponding porphyrazine complex, [FeIII(TBP8Pz)]Cl , forms diamagnetic bis-CN and bis-tBuNC under the same conditions: TBP8Pz is a dianion of 2,3,7,8,12,13,17,18-octakis(4-tert-butylphenyl)-porphyrazine. Thus, the iron(III) ion of porphyrazine complex is more easily reduced than that of the corresponding corrolazine complex.

scholarly journals Synthesis and Spectroscopic Characterization of l-Aspartic Acid Complexes with Metals of the Lanthanides Family

2013 ◽  
Vol 11 ◽  
pp. 91-115 ◽  
Author(s):  
Musa E. Mohamed
Keyword(s):  
Aspartic Acid ◽  
Spectroscopic Characterization ◽  
Downfield Shift ◽  
H Nmr ◽  
Lanthanide Series ◽  
Chiral Carbon ◽  
Metal Contents ◽  
Metal Effect ◽  
C Nmr

The complexes between l-aspartic acid and metals of lanthanide series (La3+, Pr3+, Eu3+, Gd3+) have been prepared and characterized using a variety of techniques including, infrared spectroscopy, 1H NMR, 13C NMR, elemental analysis and metal contents. The sought metal effect on the electronic environment of the chiral carbon and its neighbouring atoms was observed in case of Europium and Praseodymium. The 13C downfield shift indicates a lower electron density at the carbon with consequent downfield shift observed on the α-H attached to it increasing its acidity.

scholarly journals Electrochemical and Spectroscopic Characterization of Aluminium(III)-para-methyl-meso-tetraphenylporphyrin Complexes Containing Substituted Salicylates as Axial Ligands

2013 ◽  
Vol 2013 ◽  
pp. 1-10
Author(s):  
Gauri D. Bajju ◽  
Deepmala ◽  
Sunil Kumar Anand ◽  
Sujata Kundan ◽  
Narinder Singh
Keyword(s):  
Spectroscopic Characterization ◽  
Redox Properties ◽  
Proton Nuclear Magnetic Resonance ◽  
Spectroscopic Techniques ◽  
Axial Coordination ◽  
H Nmr ◽  
Axial Ligands ◽  
Reduction Mechanisms ◽  
C Nmr

A series of aluminium(III)-p-methyl-meso-tetraphenylporphyrin (p-CH3TPP-Al(III)) containing axially coordinated salicylate anion [p-CH3TPP-Al-X)], where X = salicylate (SA), 4-chlorosalicylate (4-CSA), 5-chlorosalicylate (5-CSA), 5-flourosalicylate (5-FSA), 4-aminosalicylate (4-ASA), 5-aminosalicylate (5-ASA), 5-nitrosalicylate (5-NSA), and 5-sulfosalicylate (5-SSA), have been synthesized and characterized by various spectroscopic techniques including ultraviolet-visible (UV-vis), infrared (IR) spectroscopy, proton nuclear magnetic resonance (1H NMR) spectroscopy,13C NMR, and elemental analysis. A detailed study of electrochemistry of all the synthesized compounds has been done to compare their oxidation and reduction mechanisms and to explain the effect of axial coordination on their redox properties.

Functional chalcone-substituted tetrakis-metallophthalocyanines: Synthesis and spectroscopic characterization

2019 ◽  
Vol 44 (3-4) ◽  
pp. 148-151
Author(s):  
Volkan Çakır
Keyword(s):  
Spectroscopic Characterization ◽  
H Nmr ◽  
Vis Spectroscopy ◽  
New Compounds ◽  
C Nmr

In this study, a new phthalonitrile derivative, ( E)-4-(3-(3-(3-methoxyphenyl)acryloyl)phenoxy)phthalonitrile, and four peripherally ( E)-4-(3-(3-(3-methoxyphenyl)acryloyl)phenoxy) tetrasubstituted new Ni(II), Zn(II), Co(II), and Cu(II) phthalocyanine derivatives are synthesized and characterized. ( E)-4-(3-(3-(3-Methoxyphenyl)acryloyl)phenoxy)phthalonitrile is synthesized by heating ( E)-1-(3-hydroxyphenyl)-3-(3-methoxyphenyl)prop-2-en-1-one and 4-nitrophthalonitrile in the presence of K2CO3 in dry DMF at 60°C for 96 h. The metallophthalocyanines are prepared by cyclotetramerization of ( E)-4-(3-(3-(3-methoxyphenyl)acryloyl)phenoxy)phthalonitrile with NiCl2, Zn(CH3COO)2, CoCl2, and CuCl2 in n-pentanol in the presence of 1,8-diazabicyclo[5.4.0]undec-7-ene. Characterization of the new compounds is performed by means of IR, 1H NMR, 13C NMR, and mass and UV-Vis spectroscopy techniques.

scholarly journals Synthesis, Characterization, and Agricultural Biological Activities of 5-Fluoro-2-hydroxy Butyrophenone

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Fengli Xin ◽  
Chunhua Du ◽  
Gongjia Lan ◽  
Zhuanping Wu
Keyword(s):  
Lactuca Sativa ◽  
Biological Activities ◽  
Raw Material ◽  
Synthetic Approach ◽  
Target Compound ◽  
Echinochloa Crusgalli ◽  
Agricultural Plant ◽  
H Nmr ◽  
Valsa Mali ◽  
C Nmr

A novel synthetic approach towards 5-fluoro-2-hydroxy butyrophenone is reported. Using 4-fluorophenol as a raw material, the processes of etherification protection, Friedel-Crafts acylation and demethylation provide the target compound under mild conditions. The structure was characterized by the melting point and IR, MS,1H-NMR, and13C-NMR spectroscopy. The bioassay results indicate that the target compound exhibits potent antifungal activities againstValsa mali,Coniella dipodiella, and other agricultural plant fungi. The target compound also shows potent herbicidal activities forLactuca sativa, a dicotyledon, andEchinochloa crus-galli, a monocotyledon. The toxicity regression C50values of the compound againstValsa mali,Coniothyrium diplodiella,Lactuca sativaseedling, andEchinochloa crusgalliseedling were calculated by SPSS. The Hormesis effect for roots ofEchinochloa crusgalliwas confirmed.

scholarly journals Structural Characterization of Amadori Rearrangement Product of Glucosylated Nα-Acetyl-Lysine by Nuclear Magnetic Resonance Spectroscopy

2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Chuanjiang Li ◽  
Hui Wang ◽  
Manuel Juárez ◽  
Eric Dongliang Ruan
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Maillard Reaction ◽  
Structural Characterization ◽  
Resonance Spectroscopy ◽  
H Nmr ◽  
Amadori Rearrangement ◽  
C Nmr ◽  
Nuclear Magnetic

Maillard reaction is a nonenzymatic reaction between reducing sugars and free amino acid moieties, which is known as one of the most important modifications in food science. It is essential to characterize the structure of Amadori rearrangement products (ARPs) formed in the early stage of Maillard reaction. In the present study, the Nα-acetyl-lysine-glucose model had been successfully set up to produce ARP, Nα-acetyl-lysine-glucose. After HPLC purification, ARP had been identified by ESI-MS with intense [M+H]+ ion at 351 m/z and the purity of ARP was confirmed to be over 90% by the relative intensity of [M+H]+ ion. Further structural characterization of the ARP was accomplished by using nuclear magnetic resonance (NMR) spectroscopy, including 1D 1H NMR and 13C NMR, the distortionless enhancement by polarization transfer (DEPT-135) and 2D 1H-1H and 13C-1H correlation spectroscopy (COSY) and 2D nuclear overhauser enhancement spectroscopy (NOESY). The complexity of 1D 1H NMR and 13C NMR was observed due to the presence of isomers in glucose moiety of ARP. However, DEPT-135 and 2D NMR techniques provided more structural information to assign the 1H and 13C resonances of ARP. 2D NOESY had successfully confirmed the glycosylated site between 10-N in Nα-acetyl-lysine and 7′-C in glucose.

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