Synthesis of 4H-chromene derivatives by reaction between alkyl isocyanides and dialkyl acetylenedicarboxylate in the presence of 6-hydroxyquinoline

The reactive intermediate generated by the addition of alkyl isocyanides to dialkyi acetyienedicarboxyiate was trapped by 6- quinolinol to produce highlyfunctionalized 4H-chromenes in fairly good yields.     

Characterisation of the dispersion in polymer flame retarded nanocomposites

Flame retardant nanocomposites have attracted many research efforts because they combine the advantages of a conventional flame retardant polymer with that of polymer nanocomposite. However the properties obtained depend on the dispersion of the nanoparticles. In this study, three types of polymer flame retarded nanocomposites based on different matrices (polypropylene (PP), polybutadiene terephtalate (PBT) and polyamide 6 (PA6)) have been prepared by extrusion. In order to investigate the dispersion of nanoparticles in the polymer containing flame retardant, conventional methods used to characterise the morphology of composites have been applied to FR composites containing nanoclays. XRD, TEM and melt rheology give useful information to describe the dispersion of the nanofiller in the flame retarded nanocomposite. In the PA6-OP1311 (phosphorus based flame retardant) materials, the clay is well dispersed unlike in PBT and PP materials where microcomposites are obtained with some intercalation. The poor dispersion is also highlighted by NMR measurements but the presence of flame retardant particles interferes in the quantitative evaluation of nanoclay dispersion and underestimations are made.     

Crossed characterisation of polymer-layered silicate (PLS) nanocomposite morphology: TEM, X-ray diffraction, rheology and solid-state nuclear magnetic resonance measurements

As the nanocomposite properties dramatically depend on the dispersion state of the filler in the matrix, it is essential to develop technical methods to characterise the nanodispersion both qualitatively and quantitatively. In this study, complete characterisations of the nanodispersion of organomodified clays in polyamide 6, polypropylene and poly(butylene terephtalate) are presented and discussed using different analytical tools. All four characterisation methods have been evaluated experimentally. TEM has been used to qualitatively characterise the dispersion. As TEM picture might be not fully representative of the whole sample, many pictures have to be analysed to mirror the global repartition. XRD is particularly adapted to the study of intercalated morphology of nanocomposite since the distance between two platelets can be calculated but needs TEM to provide more complete conclusions. Melt rheology and solid-state NMR are bulk analyses. During the measurement the sample is representative of the material. Rheology is relatively simple to make measurements and to get semi-quantitative data. In connection with NMR, we can get quantitative measurements on the degree of nanodispersion in the nanocomposite.     

Sustainable Surfactin Production by Bacillus subtilis Using Crude Glycerol from Different Wastes

Most biosurfactants are obtained using costly culture media and purification processes, which limits their wider industrial use. Sustainability of their production processes can be achieved, in part, by using cheap substrates found among agricultural and food wastes or byproducts. In the present study, crude glycerol, a raw material obtained from several industrial processes, was evaluated as a potential low-cost carbon source to reduce the costs of surfactin production by Bacillus subtilis #309. The culture medium containing soap-derived waste glycerol led to the best surfactin production, reaching about 2.8 g/L. To the best of our knowledge, this is the first report describing surfactin production by B. subtilis using stearin and soap wastes as carbon sources. A complete chemical characterization of surfactin analogs produced from the different waste glycerol samples was performed by liquid chromatography–mass spectrometry (LC-MS) and Fourier transform infrared spectroscopy (FTIR). Furthermore, the surfactin produced in the study exhibited good stability in a wide range of pH, salinity and temperatures, suggesting its potential for several applications in biotechnology.     

Facile and rapid access to inosine puromycin analogues through the use of adenylate deaminase

To study the ribosomal peptidyl transfer, puromycin analogues are of interest in which adenine has been replaced by hypoxanthine. We synthesized inosine puromycin analogues from 3'-azidodeoxyadenosine derivatives using adenylate deaminase for the quantitative transformation of the N-heterocycle. The amino acid coupling was carried out under Staudinger-Vilarrasa conditions in 94% yield starting from the protected and in 82% using the unprotected azide, thus, in the presence of two hydroxyls and a lactam function.     

First synthesis of 2'-deoxyfluoropuromycin analogues: experimental insight into the mechanism of the Staudinger reaction

The N(6),N(6)-dedimethyl-2'-deoxyfluoro analogue of puromycin (= 3'-deoxy-N(6),N(6)-dimethyl-3'-[O-methyltyrosylamido]adenosine), its 2',3'-regioisomer and a 3'-cytidyl-5'-(2'-deoxyfluoro)puromycyl dinucleotide analogue were synthesized following an approach involving i) the diastereospecific nitrite-assisted formation of a lyxo nucleosidic 2',3'-epoxide from an adenosine-2',3'-ditriflate derivative in a biphasic solvent mixture; ii) the regio- and stereoselective epoxide ring opening with sodium azide under mildly acidic aqueous conditions, iii) the stereospecific introduction of the fluor atom using DAST and iv) the reaction between the nucleosidyl or dinucleotidyl azide and an active ester of the N-protected amino acid using highly efficient solution conditions for the Staudinger-Vilarrasa coupling, to obtain the corresponding carboxamide directly from the in situ formed iminophosphorane. This coupling reaction furnished sterically quite demanding amides in 94 % isolated yields under very mild conditions and should therefore be of a more general value. Under certain reaction conditions we isolated (amino)acyltriazene derivatives from which dinitrogen was not eliminated. These secondary products are trapped and stabilized witnesses of the first intermediate of the Staudinger reaction, the phosphatriazenes (phosphazides, triazaphosphadienes) which usually eliminate dinitrogen in situ and rapidly rearrange into iminophosphoranes, unless they are derived from conjugated or sterically bulky azides and phosphines. The acyltriazenes could either be thermally decomposed or converted to the corresponding N-alkyl carboxamides through proton-assisted elimination of dinitrogen. All compounds were carefully characterized through MS spectrometry, (1)H, (19)F, (31)P and (13)C NMR spectroscopy.     

Single-point magnetic resonance imaging study of water adsorption in pellets of zeolite 4A

The water uptake process in commercial type particles of zeolite 4A has been studied using a single-point MRI method. True proton density, T1, T2, and T*2 relaxation times were obtained with submillimetric resolution, overcoming the restrictions of short T*2 signals. The molecular mobility in nonequilibrium conditions has been characterized by relaxation time mapping. A clear reduction of the water sorption rate was observed by comparing MRI profiles of a loosely packed bed and gravimetric measurements of spread particles from the same sieved zeolite batch.     

Artemisinin and Derivatives-Based Hybrid Compounds: Promising Therapeutics for the Treatment of Cancer and Malaria

Cancer and malaria are major health conditions around the world despite many strategies and therapeutics available for their treatment. The most used strategy for the treatment of these diseases is the administration of therapeutic drugs, which suffer from several shortcomings. Some of the pharmacological limitations associated with these drugs are multi-drug resistance, drug toxicity, poor biocompatibility and bioavailability, and poor water solubility. The currently ongoing preclinical studies have demonstrated that combination therapy is a potent approach that can overcome some of the aforementioned limitations. Artemisinin and its derivatives have been reported to exhibit potent efficacy as anticancer and antimalarial agents. This review reports hybrid compounds containing artemisinin scaffolds and their derivatives with promising therapeutic effects for the treatment of cancer and malaria.     

Diffusion and Immobilization Mechanisms in Zeolites Studied by ZLC Chromatography

Zero Length Column chromatography was used to study mass transfer in zeolites involving coupled diffusion and immobilization mechanisms. A modeling based on Volterra integral equation technique was utilized to simulate sorption and desorption kinetic curves and compare results of the simulations with experimentally obtained curves. This approach was applied to analyze sorption kinetics in the model system: toluene/silicalite-1 (75°C–178°C). The system generally shows a non-Fickian behavior and can be described by diffusion coupled with immobilization.An erratum to this article can be found at     

Detection of genetically modified organisms in foods by protein- and DNA-based techniques: bridging the methods

According to European Commission (EC) Regulation 1139/98, foods and food ingredients that are to be delivered to the final consumer in which either protein or DNA resulting from genetic modification is present, shall be subject to additional specific labeling requirements. Since 1994, genetically altered tomatoes, squash, potatoes, canola, cotton, and soy have been on the market. Recently, insect-resistant and herbicide-tolerant maize varieties have been introduced. Soy and maize are 2 of the most important vegetable crops in the world. During the past 4 years, both protein- and DNA-based methods have been developed and applied for detection of transgenic soy and maize, and their derivatives. For protein-based detection, specific monoclonal and polyclonal antibodies have been developed; for immunochemical detection, Western blot analysis and enzyme-linked immunosorbent assays are the most prominent examples. For detection of genetically modified organisms (GMOs) at the level of DNA, polymerase chain reaction-based methods are mainly used. For these reactions, highly specific primer sets are needed. This study compares the principally different methods. Specificity of methods and the possible risks of false-positive or false-negative results are considered in relation to sampling, matrix effects, and food processing procedures. In addition, quantitative aspects of protein- and DNA-based GM detection methods are presented and discussed. This is especially relevant as EC regulation 49/2000, which defines a threshold for an unintentional comingling of 1%, came into force on April 10, 2000.