Synthesis and Characterization of Pd{II) and Ni(II) Complexes of Schiff Bases and Catalytic Activity of Pd(II) Complexes

2015 ◽  
Vol 12 (2) ◽  
pp. 1
Author(s):  
Amalina Mohd Tajuddin ◽  
Hadariah Bahron ◽  
Shahrul Nizam Ahmad
Keyword(s):  
Coupling Reaction ◽  
Catalytic Performance ◽  
Optimum Operating ◽  
Catalyst Loading ◽  
Spectroscopic Techniques ◽  
1H And 13C Nmr ◽  
Cross Coupling Reaction ◽  
Square Planar ◽  
Ft Ir

Six new Pd(Il) and Ni(Il) metal complexes of N, O-bidentate (LI, L2) and ONNO-tetradentate (L3) Schiff base ligands have been synthesized. The compounds were characterized via various physicochemical and spectroscopic techniques namely elemental analysis (CHN), FT-IR, 1H and 13C NMR. as well as magnetic susceptibility measurement. All complexes showed diamagnetism indicating that they are square planar complexes. Catalytic performance of Pd(Ll)2 and Pd(L2)2 were investigated/or Heck cross-coupling reaction under optimum operating parameters, monitored using GC-FID for 6 h of reaction time in inert conditions. High catalytic activities of up to 90% were observed in the presence of triethylamine as base and DMA as solvent at J0()"C with I mmol% catalyst loading. The mechanism of catalyzed Heck reaction is proposed to go through a series of conversion of Pd(0)/Pd(Il).

Synthesis and Characterization of Pd(II) and Ni(II) Complexes of Schiff Bases and Catalytic Activity of Pd(II) Complexes

2015 ◽  
Vol 12 (2) ◽  
pp. 1 ◽  
Author(s):  
Amalina Mohd Tajuddin ◽  
Hadariah Bahron ◽  
Shahrul Nizam Ahmad
Keyword(s):  
Coupling Reaction ◽  
Catalytic Performance ◽  
Optimum Operating ◽  
Catalyst Loading ◽  
Spectroscopic Techniques ◽  
1H And 13C Nmr ◽  
Cross Coupling Reaction ◽  
Square Planar ◽  
Ft Ir

Six new Pd(Il) and Ni(Il) metal complexes of N, O-bidentate (LI, L2) and ONNO-tetradentate (L3) Schiff base ligands have been synthesized. The compounds were characterized via various physicochemical and spectroscopic techniques namely elemental analysis (CHN), FT-IR, 1H and 13C NMR. as well as magnetic susceptibility measurement. All complexes showed diamagnetism indicating that they are square planar complexes. Catalytic performance of Pd(L1)2 and Pd(L2)2 were investigated for Heck cross-coupling reaction under optimum operating parameters, monitored using GC-FID for 6 h of reaction time in inert conditions. High catalytic activities of up to 90% were observed in the presence of triethylamine as base and DMA as solvent at 100C with 1 mmol% catalyst loading. The mechanism of catalyzed Heck reaction is proposed to go through a series of conversion of Pd(0)/Pd(II).

Steroid Compounds Isolation from Carthamus tinctorius Linn as Antimalarial

2021 ◽  
pp. 5297-5304
Author(s):  
Rini Hamsidi ◽  
Wahyuni Wahyuni ◽  
Adryan Fristiohady ◽  
Muhammad Hajrul Malaka ◽  
Idin Sahidin ◽  
...  
Keyword(s):  
Antimalarial Activity ◽  
Carthamus Tinctorius ◽  
Spectroscopic Techniques ◽  
1H And 13C Nmr ◽  
Marker Compound ◽  
Ic50 Value ◽  
Ft Ir ◽  
Ir Spectroscopic

Carthamus tinctorius Linn, also known as safflower, is a plant with the potential of being used in the production of antimalarial drugs. The purpose of this study was to isolate and identify the steroid compounds in the safflower and determine its antimalarial activity in vitro. The isolation process was conducted through extraction and chromatography methods. Then, the characterization of the isolated compounds was conducted through spectroscopic techniques which include Fourier Transform Infrared Spectroscopy (FT-IR), NMR 1-D (1H and 13C-NMR), and NMR 2-D (HMQC, HMBC, and H-H COZY) as well as comparing data with the existing literatures. In addition, the tests conducted were with variations of isolate concentrations (10, 1, 0.1, 0.01, and 0.001 μg/mL) against 3D7 strain of Plasmodium falciparum. Based on the FT-IR spectroscopic data, the steroid compounds isolated from safflowers might be stigmasterols. In addition, the isolates had -OH functional group in the region of 3431 cm-1, C-O in the region of 1053 cm-1, and Csp3-H in regions of 2960, 2934, and 2865 cm-1. The NMR 1-D data showed presence of 29 carbon atoms, while the protons were 48 in number. Furthermore, the IC50 value of the compound was 34.03 μg/mL with a percentage inhibition of 43.92% against the growth of P. falciparum. Therefore, it was classified as inactive agent in inhibiting the growth of malaria parasites, however, it could be used as a marker compound in C. tinctorius Linn extract.

scholarly journals Pd(II) Complexes with Nitrogen-oxygen Donor Ligands: Synthesis, Characterization and Catalytic Activity for Suzuki-Miyaura Cross-coupling Reaction

2014 ◽  
Vol 31 (1) ◽  
pp. 15
Author(s):  
M.T Amalina ◽  
B Hadariah ◽  
K Karimah ◽  
W.I.W Nazihah
Keyword(s):  
Phenylboronic Acid ◽  
Coupling Reaction ◽  
Cross Coupling ◽  
Donor Ligands ◽  
Azomethine Nitrogen ◽  
Catalyst Loading ◽  
Cross Coupling Reaction ◽  
Oxygen Donor ◽  
Counter Ions ◽  
Square Planar

Inexpensive bidentate Schiff base ligands (O1, O3) and their Pd(II) complexes (OPd1, OPd3) were successfully synthesized and characterized using CHN elemental analysis, FTIR, 1H and 13C NMR, melting point determination, molar conductivity and magnetic moment. It revealed that these Schiff bases behaved as bidentate ligands in their complexes. The spectral data indicated that the ligands co-ordinated through the phenolic oxygen and the azomethine nitrogen atoms. Magnetic momentdata suggested the existence of square planar Pd(II) complexes, while non-electrolytic behaviour indicated the absence of counter ions in chloroform. The Pd(II) complexes showed good catalytic activities for Suzuki-Miyaura cross-coupling reaction between iodobenzene with phenylboronic acid at 1.0 mmol% catalyst loading.

scholarly journals Tetradentate Palladium(II) Salophen Complexes: Synthesis, Characterization and Catalytic Activities in Copper-Free Sonogashira Coupling Reaction

2018 ◽  
Vol 7 (3.11) ◽  
pp. 15 ◽  
Author(s):  
Shahrul Nizam Ahmad ◽  
Hadariah Bahron ◽  
Amalina Mohd Tajuddin
Keyword(s):  
Condensation Reaction ◽  
Coupling Reaction ◽  
13C Nmr Spectroscopy ◽  
Insertion Reaction ◽  
Catalyst Loading ◽  
Sonogashira Coupling ◽  
1H And 13C Nmr ◽  
Catalytic Activities ◽  
Sonogashira Coupling Reaction

This paper reports the synthesis and characterization of three salophen ligands; 2,2'-((1E,1'E)-(1,2 phenylenebis(azanylylidene))bis(methanylylidene))diphenol [L1H], 2,2'-((1E,1'E)-(1,2-phenylenebis(azanylylidene))bis (methanylylidene))bis(4-chlorophenol) [L1C] and 2,2'-((1E,1'E)-(1,2-phenylenebis(azanylylidene))bis(methanylylidene))bis(4-methoxylphenol) [L1OME]. The compounds were prepared from condensation reaction between salicylaldehyde, and its derivatives, with ortho-phenylenediamine. Their palladium(II) complexes, namely PdL1H, PdL1C and PdL1OME were synthesized through insertion reaction between the ligands with palladium(II) acetate. All compounds were characterized through melting point, elemental analysis, infrared spectroscopy, 1H and 13C NMR spectroscopy. Palladium(II) complexes were tested as homogenous catalysts in copper-free Sonogashira coupling reaction between iodobenzene and phenylacetylene in DMSO using triethylamine as base with 1.0 mmol% catalyst loading. The most performing catalyst was PdL1OME with 91% conversion followed by PdL1H (83%) and PdL1C (27%).   

Supported Palladium Catalysis Using a Biguanide N-Donor Motif on Mesoporous Silica for Suzuki-Miyaura Coupling Reaction

2012 ◽  
Vol 622-623 ◽  
pp. 757-761
Author(s):  
Amirhossein Fallah ◽  
Davood Kordestani ◽  
Abdolhamid Alizadeh ◽  
Salasiah Endud
Keyword(s):  
Palladium Catalysis ◽  
Coupling Reaction ◽  
Surface Characteristics ◽  
Catalytic Performance ◽  
Cross Coupling Reaction ◽  
Ordered Mesoporous ◽  
Recoverable Catalyst ◽  
Ft Ir ◽  
Supported Palladium ◽  
Supported Pd

A supported Pd(II)/biguanide complex on ordered mesoporous SBA-15 material (Pd@SBA-15/Met) exhibited catalytic activity in the cross-coupling reaction. The structural and surface characteristics of the prepared catalysts were investigated by various techniques (XRD, SEM, FT-IR and AAS). The catalytic performance of the catalysts was evaluated in Suzuki-Miyaura coupling reaction and it was proved to act as a recoverable catalyst in green media with excellent reactivity combined with recyclability.

scholarly journals Synthesis and Structural Characterization of (E)-4-[(2-Hydroxy-3-methoxybenzylidene)amino]butanoic Acid and Its Novel Cu(II) Complex

Molbank ◽  
10.3390/m1179 ◽  
2021 ◽  
Vol 2021 (1) ◽  
pp. M1179
Author(s):  
Eleftherios Halevas ◽  
Antonios Hatzidimitriou ◽  
Barbara Mavroidi ◽  
Marina Sagnou ◽  
Maria Pelecanou ◽  
...  
Keyword(s):  
Schiff Base ◽  
Gamma Aminobutyric Acid ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
Polymeric Compound ◽  
Bridging Ligands ◽  
1H And 13C Nmr ◽  
One Dimensional ◽  
Ft Ir

A novel Cu(II) complex based on the Schiff base obtained by the condensation of ortho-vanillin with gamma-aminobutyric acid was synthesized. The compounds are physico-chemically characterized by elemental analysis, HR-ESI-MS, FT-IR, and UV-Vis. The complex and the Schiff base ligand are further structurally identified by single crystal X-ray diffraction and 1H and 13C-NMR, respectively. The results suggest that the Schiff base are synthesized in excellent yield under mild reaction conditions in the presence of glacial acetic acid and the crystal structure of its Cu(II) complex reflects an one-dimensional polymeric compound. The molecular structure of the complex consists of a Cu(II) ion bound to two singly deprotonated Schiff base bridging ligands that form a CuN2O4 chelation environment, and a coordination sphere with a disordered octahedral geometry.

scholarly journals GREEN SYNTHESIS AND SPECTROSCOPIC CHARACTERIZATION OF IRON (III) COMPLEX OF UREA FROM HUMAN URINE AND IRON RUST

2020 ◽  
Vol 45 (5) ◽  
Author(s):  
V.O. Uduah ◽  
J.J. Gongden ◽  
M.L. Kagoro ◽  
K.K. Gurumyen ◽  
Y.N. Lohdip ◽  
...  
Keyword(s):  
Human Urine ◽  
Synthesis Method ◽  
Reaction Medium ◽  
Spectroscopic Characterization ◽  
Waste Materials ◽  
Spectroscopic Techniques ◽  
Distilled Water ◽  
Oxide Composition ◽  
Ft Ir

This work presents a dry synthesis of Iron (III) complex with urea isolated from human urine and Fe (III) obtained from iron rust particles. Iron (III), PI (Purified iron rust), was isolated from iron rust in 10% hydrochloric acid, HCl and distilled water respectively. The complex was synthesized via dry-synthesis method using the melted urea as reaction medium. The isolated Fe (III) was characterized by elemental analysis which was done using XRF Cu-Zn method. The complex was prepared in a 1:4 metal to ligand (M-L) ratio. The stoichiometry of reaction indicate a 1:3 ratio of M-L (Fe-U). The complex was characterized by FT-IR, UV-vis, XRF and XRD spectroscopic techniques. The Fe (III) isolate and Fe-U complex shows percentage yields of 35.7% and ~92% respectively. The elemental and oxide composition of Fe and Fe2O3 (i.e., PI) were 40.387% and 57.753% respectively. The results obtained from the characterization of the iron-urea complex, IUC, indicate FT-IR result as symmetric and asymmetric frequencies with peaks of a combination band of Vs (NH) and Vas (NH), C=O and V (C-N) all stretched, XRD showed the crystal to be amorphous. The elemental and oxide composition of the Fe and Fe2O3 in IUC were 40.007 and 44.201 respectively. The results obtained revealed that useful complexes can be synthesized easily from waste materials, such as urine and iron rust particles, which complement Green chemistry.

scholarly journals Synthesis and Characterization of 2-Pyrazoline Derivatives and their in silico and in vitro Studies on Antimicrobial and Anticancer Activities

2019 ◽  
Vol 31 (10) ◽  
pp. 2191-2196 ◽  
Author(s):  
S. Rathinamanivannan ◽  
K. Megha ◽  
Raja Chinnamanayakar ◽  
Ashok Kumar ◽  
M.R. Ezhilarasi
Keyword(s):  
Breast Cancer ◽  
Synthesis And Characterization ◽  
Anticancer Activities ◽  
1H And 13C Nmr ◽  
Chemical Structures ◽  
Ft Ir ◽  
Affinity Score ◽  
High Binding Affinity

The new series of 1-(4,5-dihydro-5-phenyl-3-diphenylpyrazol-1-yl)butan-1-one derivatives were synthesized by cyclization method using biphenyl chalcone with n-butyric acid and hydrazine hydrate. The synthesized 1-(4,5-dihydro-5-phenyl-3-diphenylpyrazol-1-yl)butan-1-one derivatives chemical structures were confirmed from spectral data such as FT-IR, 1H and 13C NMR. 2-Pyrazoline derivatives were docked with bacterial (1UAG) and breast cancer (1OQA) protein. Based on high binding affinity score, the best compound was subjected to in vitro anticancer activity by MTT assay. Also, antimicrobial activity were studied for synthesized 2-pyrazoline derivatives.

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