MK-10 Clay–Catalyzed Synthesis of 2-(2′,5′-Disubstituted-1′H-indol-3′-yl)-1H-benzo[d]imidazoles under Conventional and Microwave Irradiation

The synthesis of benzimidazoles has been achieved in a one-pot reaction in excellent yield using a newly developed methodology. 2,5-Disubstituted-3-cyanoacetyl indoles were directly condensed with substituted orthophenylenediamine via microwave irradiation under neat, solid support, and conventional conditions in a short time to afford the corresponding products in good yields. Structures of the products thus obtained were confirmed by their melting points, infrared, ¹H NMR, ¹³C NMR, and mass spectral data.

Microwave‐Assisted Synthesis and Antiprotozoal Activity of Pyridazines Carrying Polyfluoro Substituents

A number of 4,5‐dichloro‐ and 4,5‐dibromopyridazin‐3‐ones and ‐3,6‐diones with polyfluoro substituents at position 2 were obtained in good yields by microwave‐assisted method. The oxopyridazines as well as their respective 5‐dimethylaminoethylamino derivatives were tested for antibacterial, antiviral, and antiprotozoal activity.     

Multicomponent Reaction for Synthesis of 2-(Indol-3-yl)pyridine Derivatives Under Microwave Irradiation

A short, practical, and efficient preparation of 2-(indol-3-yl)pyridine derivatives via a one-pot procedure of 3-cyanoacetylindole, chalcones, and ammonium acetate under microwave irradiation was described. All these compounds were obtained in good yield, and their structures were confirmed by ¹H NMR, infrared, and elementary analysis.      

Improved Synthesis of 1-Bromo-3-buten-2-one

A convenient procedure for the synthesis of 1-bromo-3-buten-2-one, 4, from commercially available 2-ethyl-2-methyl-1,3-dioxolane, 1, is described. The procedure involves three reaction steps: (1) The acetal 1 is converted to 2-(1-bromoethyl)-2-bromomethyl-1,3-dioxolane, 2, by reacting 1 with elemental bromine in dichloromethane to yield 98% of 2. (2) Dehydrobromination of 2 with potassium tert-butoxide in tetrahydrofuran gives 2-bromomethyl-2-vinyl-1,3-dioxolane, 3, in 84–93% yield. (3) Removal of the acetal protection from 3 by formolysis for 6–10 h afforded 1-bromo-3-buten-2-one, 4, in 85–94% yield. A more rapid method is acid hydrolysis of 3 under microwave activation (100 °C, 8–10 min), by which 4 was obtained in 75% yield. Full experimental details are given.

Rapid Conventional and Microwave-Assisted Decarboxylation of L-Histidine and Other Amino Acids via Organocatalysis with R-Carvone Under Superheated Conditions

This article reports a new methodology taking advantage of superheated chemistry via either microwave or conventional heating for the facile decarboxylation of alpha amino acids using the recoverable organocatalyst, R-carvone. The decarboxylation of amino acids is an important synthetic route to biologically active amines, and traditional methods of amino acid decarboxylation are time consuming (taking up to several days in the case of L-histidine), are narrow in scope, and make use of toxic catalysts. Decarboxylations of amino acids including L-histidine occur in just minutes while replacing toxic catalysts with green catalyst, spearmint oil. Yields are comparable to or exceed previous methods and purification of product ammonium chloride salts is aided by an isomerization reaction of residual catalyst to phenolic carvacrol. The method has been shown to be effective for the decarboxylations of a range of natural, synthetic, and protected amino acids.     

Microwave-Assisted Chemical Demulsification of Water-in-Crude-Oil Emulsions

Two case studies are presented that shows the effects of chemical demulsifiers used under conventional heating and in combination with microwave radiation on efficiency of demulsification and light transmittance of the water separated from the emulsions. The data shows that the chemical demulsifiers coupling with microwave radiation does a better job at demulsifying the water-in-crude-oil emulsions than when the chemical demulsifiers are used under conventional heating. The demulsification efficiency of AE-121 could reach 100% under microwave irradiation (300 W) for 50 seconds.     

Thermal Stabilities of Attapulgite/Polystyrene (ATP/PS) Nanocomposites via Microwave‐Assisted Bulk Polymerization

Attapulgite/polystyrene (ATP/PS) nanocomposites with different contents of attapulgite nano‐needles organo‐modified, and cetyltrimethylammonium bromide (CTAB) were successfully prepared by the in situ bulk radical polymerization of styrene, under microwave irradiation. The transmission electron microscopy (TEM) results showed good dispersibility of the organo‐modified attapulgite nano‐needles in the polystyrene matrices. The thermogravimetric analysis (TGA) revealed that the thermal stability of the nanocomposite was enhanced with the increase of additional attapulgite nano‐needles.     

Microwave‐Assisted Synthesis and Characterization of CuO Nanocrystals

CuO feather‐like and flower‐like crystals have been synthesized by a fast microwave‐assisted solution approach using Cu(NO₃)₂ and NaOH. The morphology transformation of CuO could be achieved by ionic liquid 1‐n‐butyl‐3‐methyl imidazolium tetrafluoroborate ([BMIM]BF₄). With [BMIM]BF₄, flower‐like CuO were obtained, whereas without [BMIM]BF₄, feather‐like CuO were obtained. The possible formation mechanism of flower‐like CuO was discussed on the basis of experimental results. The products were characterized by XRD, FESEM/EDS, and TEM/SAED. In addition, the adsorption of [BMIM]BF₄ on flower‐like CuO was confirmed by FTIR and TG/DSC, and the band gap energies of the flower‐like CuO was estimated by UV‐vis spectra.     

Application of a new focused microwave technology with species-specific isotope dilution analysis for the quantitative extraction of organometallic contaminants in solid environmental matrices

A new self-tuning single-mode-focused microwave technology has been evaluated in this work to perform the quantitative routine extraction of organometallic species from solid matrices of environmental interest. Species-specific isotope dilution analysis has been employed to better investigate the real influence of the microwave-assisted extractions on the final results. The advantages of such methodology in comparison with other established microwave units for the routine speciation analysis of organomercury and organotin compounds are discussed (such as the capability of using disposable glass vials, a self-tuning mode to provide an accurate control of the temperature and pressure inside of the vials, and the possibility of performing automated sequence of extractions with low sample size). The results obtained in this work demonstrated that such technology provides a fast and reliable quantitative extraction of the organometallic species in a wide range of extraction conditions even when the multi-elemental (Sn and Hg) species-specific determination is carried out.     

Design and Synthesis of a γ1β8‐Cyclodextrin Oligomer: A New Platform with Potential Application as a Dendrimeric Multicarrier

We report the synthesis and characterization of a water‐soluble, star‐shaped macromolecular platform consisting of eight β‐cyclodextrin (β‐CD) units anchored to the narrower rim of a γ‐CD core through bis(triazolyl)alkyl spacers. The efficient synthetic protocol is based on the microwave (MW)‐promoted Cu‐catalyzed 1,3‐dipolar cycloaddition of CD monoazides to CD monoacetylenes. The ligand‐hosting capability of the construct has been assessed by relaxometric titration and nuclear magnetic relaxation dispersion (NMRD) profiling, which showed it to be good, and this was supported by molecular dynamics simulations. To demonstrate the feasibility of obtaining supramolecular structures with high hosting ability, we designed a dimeric platform, formed by joining two nonamers through the γ‐CD cores through a bis(lithocholic acid) linker. With a view to the potential biological applications, cytotoxicity and extent of binding to human serum albumin were assessed. The properties of this dendrimeric multicarrier make it suitable for pharmaceutical and diagnostic purposes, ranging from targeted drug delivery to molecular imaging.