scholarly journals Microwave-Assisted Synthesis and Characterization of Certain Oximes, Hydrazones, and Olefins Derived fromβ-Keto Sulfones

2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Hatem A. Abdel-Aziz ◽  
Hazem A. Ghabbour ◽  
Mashooq A. Bhat ◽  
Hoong-Kun Fun

A new series ofβ-keto sulfone derivatives containing oximes4a–e, hydrazones5a, b, and chalcones7a–dwere prepared using microwave irradiation (MWI) by the reaction ofβ-keto sulfones3with hydroxyl amine, hydrazines, and aromatic aldehydes, respectively. The comparative study between microwave irradiation and conventional syntheses showed that MWI is effective in the synthesis of the title compounds through shortening of the reaction time and improvements in their yields. The structures of the synthesized compounds were established under the basis of their spectral data and X-ray single crystal analysis of compound5a. The crystal of5abelongs to triclinic space groupP-1, witha=5.7735   (2) Å,b=9.3224   (3) Å,c=13.1696   (5) Å,α=76.411   (1)°,β=89.571   (1)°,γ=79.9380   (9)°,Z=2,   V=677.97   (4) Å3,Dc=1.513 Mg m−3,μ=0.44 mm−1,F(000)=320,R=0.026, andwR=0.070for 2690 observed reflections withI>2σ(I).

2018 ◽  
Vol 73 (12) ◽  
pp. 999-1003 ◽  
Author(s):  
Mohammad Hakimi ◽  
Homeyra Rezaei ◽  
Keyvan Moeini ◽  
Heidar Raissi ◽  
Vaclav Eigner ◽  
...  

AbstractA new cyclotriphosphazene, 2,2,4,4,6,6-hexakis (o-tolylamono)-1,3,5,2λ5,4λ5,6λ5-triazatriphosphinine (MPAP), was prepared using microwave irradiation and identified by elemental analysis, FT-IR, Raman, 31P NMR spectroscopy, and single-crystal X-ray diffraction. In the crystal, in addition to hydrogen bonds, the network is further stabilized by inter- and intramolecular π–π stacking interactions between aromatic rings.


2010 ◽  
Vol 93-94 ◽  
pp. 643-646
Author(s):  
Pusit Pookmanee ◽  
Supasima Makarunkamol ◽  
Sakchai Satienperakul ◽  
Jiraporn Kittikul ◽  
Sukon Phanichphant

Zinc oxide micropowder was synthesized by a microwave-assisted method. Zinc nitrate and ammonium hydroxide were used as the starting precursors with the mole ratio of 1:1. The white precipitated powder was formed after adding ammonium hydroxide until the pH of final solution was 9 and treated with the microwave radiation power at 1000 Watt for 2-6 min. The phase of zinc oxide micropowder was examined by X-ray diffraction (XRD). A single phase of hexagonal structure was obtained. The morphology and chemical composition of zinc oxide micropowder were investigated by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The particle was plate-like in shape with the range of particle size of 0.1-0.5 µm. The elemental composition of zinc oxide showed the characteristic X-ray energy value as follows: zinc of Lα = 1.012 keV, Kα = 8.630 keV and Kβ = 9.570 keV and oxygen of Kα = 0.525 keV, respectively.


2008 ◽  
Vol 86 (5) ◽  
pp. 435-443 ◽  
Author(s):  
Francesca M Kerton ◽  
Stacey Holloway ◽  
Angela Power ◽  
R Graeme Soper ◽  
Kristina Sheridan ◽  
...  

Pure amine-bis(phenol) ligands are readily accessible in high yield, often >90%, when the Mannich condensation reactions are performed “on water” or in poly(ethyleneglycol) (PEG). Microwave-assisted synthesis dramatically reduces the time and energy required to prepare these molecules, typically from 24 h to 5 min. The approach seems to be widely applicable (7 amines and 5 phenols were tested to yield a diverse set of bis(phenol) ligands). Significant improvements in yield were observed for ligands derived from di-tert-amyl and di-tert-butyl phenols, possibly resulting from a hydrophobic effect. Single crystal X-ray diffraction data for the ligand derived from p-cresol and N,N′-dimethylethylenediamine is reported.Key words: amine-phenol, Mannich condensation, on water, microwave, ligand, high-throughput.


2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Sheauly Khatun ◽  
M. Z. H. Khan ◽  
Khodeza Khatun ◽  
M. A. Sattar

An efficient synthesis of arylidene acetophenones have been achieved by using the microwave heating in comparison to the conventional heating. In this work compound 1-phenyle-3-(4-droxyphenyle)-2-propen-1-one, 1-(4-chlorophenyle)-3-phenyle-2-propen-1-one, and 1-(4-chlorophenyle)-3-(4-hydroxyphenyle)-2-propen-1-one have been synthesized by the condensation reaction between aromatic aldehydes and substituted acetophenones under microwave irradiation. The compounds of aldehydes and acetophenones were used as benzaldehyde, parahydroxybenzaldehyde, acetophenone, and parachloroacetophenone. The result shows that the time taken for the reaction was reduced from the conventional 1-2 hours to 60–120 seconds. The yield of the compounds in the conventional heating was moderate while the highest yield of 90–98% was observed in MWI method. The structure of the compounds was characterized by their IR,1H-NMR spectral data.


2011 ◽  
Vol 10 (03) ◽  
pp. 413-418 ◽  
Author(s):  
ARUP ROY ◽  
JAYANTA BHATTACHARYA

Calcium oxide ( CaO ) is an important inorganic compound, which is used across various industries as catalyst, toxic-waste remediation agent, adsorbent, etc. CaO nanoparticles were obtained by the microwave irradiation technique, using Ca(NO3)2 ⋅ 4H2O and NaOH as starting materials. The formation of monocrystalline CaO nanoparticles was confirmed by the XRD (X-ray diffraction) and TEM (transmission electron microscopy) as well as by SAED (selected area electron diffraction) analysis. The structure of the CaO nanocrystal was found to be cubic with particle size, 24 nm and surface area, 74 m2/g.


2011 ◽  
Vol 8 (2) ◽  
pp. 945-951 ◽  
Author(s):  
P. Y. Pawar ◽  
P. M. Gaikwad ◽  
P. H. Balani

The reaction of resorcinol with ethylacetoacetate yielded the 7-hydroxy-4-methyl coumarin (1), which on treatment with benzidine gives 1-(4ʹ-amino-biphenyl-4-yl)-7-hydroxy-4-methyl-1H-quinolin-2-one (2). 1-{4ʹ-[(Substituted benzylidene)-amino]-biphenyl-4-yl}-7-hydroxy-4-methyl-1H-quinolin-2-one (3a-j) were obtained by reacting 1-(4ʹ-amino-biphenyl-4-yl)-7-hydroxy-4-methyl-1H-quinolin-2-one (2) with different substituted aromatic aldehydes in presence of glacial acetic acid by microwave irradiation. The compound 1-{4ɴ-[(substituted benzylidene)-amino]-biphenyl-4-yl}-7-hydroxy-4-methyl-1H-quinolin-2-one (3a-j) on cyclization with chloro acetyl chloride in presence of triethylamine as catalyst under microwave irradiation furnished 1-{4ʹ-[3-chloro-2-(substituted phenyl)-4-oxo-azetidin-1-yl]-biphenyl-4-yl}-7-hydroxy-4-methyl-1H-quinolin-2-one (4a-j). Purity of synthesized compounds was checked by TLC and the structures were elucidated by their IR,1H NMR, Mass and elemental analysis data. The synthesized compounds were screened for anticonvulsant activity.


2013 ◽  
Vol 2013 ◽  
pp. 1-11 ◽  
Author(s):  
Gastón P. Barreto ◽  
Graciela Morales ◽  
Ma. Luisa López Quintanilla

The effect of different variables (precursor reagents, temperature, irradiation time, microwave radiation power, and additives addition) on the final morphology of nano-ZnO obtained through the microwave assisted technique has been investigated. The characterization of the samples has been carried out by field emission scanning electron microscopy (FE-SEM) in transmission mode, infrared (FTIR), UV-Vis spectroscopy, and powder X-ray diffraction (XRD). The results showed that all the above-mentioned variables influenced to some extent the shape and/or size of the synthetized nanoparticles. In particular, the addition of an anionic surfactant (sodium di-2-ethylhexyl-sulfosuccinate (AOT)) to the reaction mixture allowed the synthesis of smaller hexagonal prismatic particles (100 nm), which show a significant increase in UV absorption.


Author(s):  
Hadis Khodadad ◽  
Farhad Hatamjafari ◽  
Khalil Pourshamsian ◽  
Babak Sadeghi

Aim and Objective: Microwave-assisted condensation of acetophenone 1 and aromatic aldehydes 2 gave chalcone analogs 3, which were cyclized to pyrazole derivatives 6a-f via the reaction with hydrazine hydrate and oxalic acid in the presence of the catalytic amount of acetic acid in ethanol. Materials and Methods: The structural features of the synthesized compounds were characterized by melting point, FT-IR, 1H, 13C NMR and elemental analysis. Results: The antibacterial activities of the synthesized pyrazoles was evaluated against three gram-positive bacteria such as Enterococcus durans, Staphylococcus aureus, Bacillus subtilis and two gram-negative bacteria such as Escherichia coli and Salmonella typhimurium. Conclusion: All the synthesized pyrazoles showed relatively high antibacterial activity against S. aureus strain and none of them demonstrated antibacterial activity against E. coli.


2020 ◽  
Vol 7 (3) ◽  
pp. 183-195
Author(s):  
Musa Özil ◽  
Emre Menteşe

Background: Benzoxazole, containing a 1,3-oxazole system fused with a benzene ring, has a profound effect on medicinal chemistry research owing to its important pharmacological activities. On the other hand, the benzoxazole derivative has exhibited important properties in material science. Especially in recent years, microwave-assisted synthesis is a technique that can be used to increase diversity and quick research in modern chemistry. The utilization of microwave irradiation is beneficial for the synthesis of benzoxazole in recent years. In this focused review, we provide a metaanalysis of studies on benzoxazole in different reaction conditions, catalysts, and starting materials by microwave technique so far, which is different from conventional heating. Methods: Synthesis of different kind of benzoxazole derivatives have been carried out by microwave irradiation. The most used method to obtain benzoxazoles is the condensation of 2-aminophenol or its derivatives with aldehydes, carboxylic acids, nitriles, isocyanates, and aliphatic amines. Results: Benzoxazole system and its derivatives have exhibited a broad range of pharmacological properties. Thus, many scientists have remarked on the importance of the synthesis of different benzoxazole derivatives. Conventional heating is a relatively inefficient and slow method to convey energy in orientation to the reaction medium. However, the microwave-assisted heating technique is a more effective interior heating by straight coupling of microwave energy with the molecules. Conclusion: In this review, different studies were presented on the recent details accessible in the microwave- assisted techniques on the synthesis of the benzoxazole ring. It presents all examples of such compounds that have been reported from 1996 to the present. Benzoxazoles showed an extensive class of chemical substances not only in pharmaceutical chemistry but also in dyestuff, polymer industries, agrochemical, and optical brighteners. Thus the development of fast and efficient achievement of benzoxazoles with a diversity of substituents in high yield is getting more noteworthy. As shown in this review, microwave-assisted synthesis of benzoxazoles is a very effective and useful technique.


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