Convenient Synthesis of 2-Aminothiophene Derivatives by Acceleration of Gewald Reaction Under Ultrasonic Aqueous Conditions

Under ultrasound irradiation and in the presence of H₂O/Et₂NH, ethyl cyanoacetate or malononitrile can combine with α-methylene carbonyl compounds and elemental sulfur to efficiently yield 2-aminothiophene derivatives within a few minutes. Products are easily obtained by simple filtration because of their spontaneous precipitation in the reaction mixtures.     

One-Pot,Three-Component Coupling Reaction: Catalyst-Free Green Synthesis of Novel N-Heteroaryl α-Naphthylglycines

A series of novel N-heteroaryl α-arylglycines containing naphthol rings has been prepared by one-pot, three-component condensation reaction of glyoxalic acid, heteroaryl amines and naphthols in water at ambient temperature and under reflux conditions in moderate to high yields. The promising advantages such as removal of organic solvent, no need to catalyst, simplicity of the reaction procedure and easy product separation will be discussed in this article.     

Aluminum Chloride (Alcl3) Promotes Selective Oxidative Deprotection of Benzylic Trimethylsilyl and Tert- Butyldimethylsilyl Ethers to the Corresponding Carbonyl Compounds with Manganese Dioxide (Mno2)

Various types of trimethylsilyl and tert-butyldimethylsilyl ethers of primary and secondary benzylic alcohols could be selectively converted to their corresponding carbonyl compounds with MnO₂ in the presence of AlCl₃ in good to excellent yields.     

Diammonium Hydrogen Phosphate: An Efficient and Versatile Catalyst for the One‐Pot Synthesis of Tetrahydrobenzo[b]pyran Derivatives in Aqueous Media

Diammonium hydrogen phosphate was used as a mild, efficient, neutral, and cheap catalyst for the synthesis of various 4H‐benzo[b]pyran derivatives via a one‐pot, three‐component condensation of aromatic aldehydes, active methylene compounds, and dimedone in aqueous media.     

Characterization of Chitosan/Alginate Self-Assembled Nanoparticles as a Protein Carrier

The aim of this study was to evaluate the effect of the polymeric ratios on the characteristics of chitosan/alginate (ch/alg) self-assembled nanoparticles and their potential as protein delivery vehicle. The nanoparticles were prepared using proper mixing of polymers in presence or absence of bovine serum albumin (BSA) as a protein model. Three formulations of nanoparticles comprising ch/alg ratios of 2:1, 1:1, and 1:2 were prepared. Size, shape and zeta potential of the formulations were studied by scanning electron microscopy (SEM) and nanosizer instruments. FTIR, and differential scanning calorimetery (DSC) studies were performed to investigate polymer-polymer or polymer-protein interactions. Release profiles and entrapment efficiencies of the nanoparticles were determined by calorimetric technique using appropriate techniques. Entrapment efficiency was 70% for ch/alg ratio of 1:1, 65% for 1:2, and 60% for 2:1. The z-average size of the nanoparticles were 403, 205, and 318 nm for ch/alg ratios of 2:1, 1:1, and 1:2, respectively. Average zeta potentials were ?47, +15, ?25 mV for 2:1, 1:1, and 1:2 as well. Considering the favorable features required for protein delivery systems, ch/alg (1:1) due to its smallest size, highest loading, and most homogenous shape was regarded as the best ratio.     

In Silico and Experimental Characterization of Chimeric Bacillus thermocatenulatus Lipase with the Complete Conserved Pentapeptide of Candida rugosa Lipase

Lipases are one of the highest value commercial enzymes as they have broad applications in detergent, food, pharmaceutical, and dairy industries. To provide chimeric Bacillus thermocatenulatus lipase (BTL2), the completely conserved pentapeptide (¹¹²Ala-His-Ser-Gln-Gly¹¹⁶) was replaced with similar sequences (²⁰⁷Gly-Glu-Ser-Ala-Gly²¹¹) of Candida rugosa lipase (CLR) at the nucleophilic elbow region. For this purpose, three mutations including A112G, H113E, and Q115A were inserted in the conserved pentapeptide sequence of btl2 gene. Based on the crystal structures of 2W22, the best structure of opened form of the chimeric lipases were garnered using the MODELLER v9.10 software. The native and chimeric lipases were docked to a set of ligands, and a trial version of Molegro Virtual Docker (MVD) software was used to obtain the energy values. Docking results confirmed chimeric lipase to be better than the native lipase. Following the in silico study, cloning experiments were conducted and expression of native and chimeric btl2 gene in Pichia pastoris was performed. The native and chimeric lipases were purified, and the effect of these mutations on characteristics of chimeric lipase studied and then compared with those of native lipase. Chimeric lipase exhibited 1.6-fold higher activity than the native lipase at 55 °C. The highest percentage of both lipases activity was observed at 60 °C and pH of 8.0. The ion Ca²⁺ slightly inhibited the activity of both lipases, whereas the organic solvent enhanced the lipase stability of chimeric lipase as compared with the native lipase. According to the results, the presence of two glycine residues at the conserved pentapeptide region of this chimeric lipase (¹¹² Gly-Glu-Ser-Ala-Gly ¹¹⁶) may increase the flexibility of the nucleophilic elbow region and affect the enzyme activity level.     

Effect of Phosphate on Glucosamine Production by Ethanolic Fungus Mucor indicus

In this study, the effect of phosphorous compound concentration on the production of glucosamine by Mucor indicus was investigated. Changes in the yield of ethanol, the major metabolite of the fungus, were also followed besides. The alkali insoluble material of the biomass of the fungus mainly contained phosphates and polymers of glucosamine and N-acetyl glucosamine, i.e., chitin and chitosan. Yields of glucosamine (78–113 g/kg dry fungal biomass) and ethanol (200–370 g/kg glucose) were significantly affected by the phosphorous concentration. The results showed that lower concentrations of phosphorous favored the production of glucosamine while higher ethanol as well as biomass yields was obtained at higher concentrations. The best concentration was 0.5 g/l where glucosamine yield was 0.37 g/l (11 % of the biomass). At this phosphate concentration, ethanol and biomass yields were 360 and 76 g/kg glucose, respectively. On average, proteins comprised 51.5 % of the biomass. Glycerol was the second important metabolite during the fermentation by the fungus which appeared at lower yields (20–34 g/kg glucose).     

Ligandless-ultrasound-assisted emulsification microextraction followed by inductively coupled plasma-optical emission spectrometry for simultaneous determination of heavy metals in water samples

In this study, a simple and efficient method of ligandless-ultrasound-assisted emulsification microextraction (LL-USAEME) followed by inductively coupled plasma-optical emission spectrometry (ICP-OES) has been developed for simultaneous extraction, preconcentration and determination of manganese, cadmium, cobalt and nickel in water samples. In the proposed approach, tetrachloroethylene was selected as extraction solvent. The effect of important experimental factors such as volume of extraction solvent, pH, sonication time, salt concentration, and temperature was investigated by using a fractional factorial design (2^5?1) to identify important factors and their interactions. In the next step, a Box-Behnken design (BBD) was applied for optimisation of significant factors. The obtained optimal conditions were: 30?µL for extraction solvent, 12 for pH, 5?min for sonication time, and 5% w/v for salt concentration. The limits of detections (LODs) for Cd(II), Co(II), Mn(II) and Ni(II) were 0.20, 0.13, 0.21 and 0.28?µg?L^?1, respectively. Relative standard deviations (RSD, C?=?200.0?µg?L^?1, n?=?9) were between 3.4–7.5% and the calibration graphs were linear in the range of 0.25 to 1000.0?µg?L^?1 for Mn, 0.5–1000.0?µg?L^?1 for Co and Ni and 1.0–250.0?µg?L^?1 for Cd. The determination coefficients (R ²) of the calibration curves for the analytes were in the range of 0.993 to 0.999. The proposed method was validated by using two certified reference materials, and also the method was applied successfully for the determination of heavy metals in different real water samples.     

Analysis of xylene in aqueous media using needle‐trap microextraction with a carbon nanotube sorbent

This paper describes a new extraction technique with needles and a sorbent based on carbon nanotubes to analyze trace amounts of three isomers of xylenes in aqueous samples. In this research, results have been compared with one commercial sorbent. The synthesized sorbent was prepared using sol–gel technology and was packed into 20 gauge needles, and the same size needle was used for packing the commercial sorbent. In the extraction process, a purge and trap sampling methodology is developed, so purging and trapping cycles were performed by a sampling pump. Optimized conditions for standard xylene samples have been obtained, and eight urine samples from workers that were exposed to xylene in the workplace were collected and analyzed. Experimental parameters such as limits of detection and quantification were investigated, and these two parameters were <1 μg/L.     

Sol–gel derived LaFeO3/SiO2 nanocomposite: synthesis,characterization and its application as a new,green and recoverable heterogeneous catalyst for the efficient acetylation of amines,alcohols and phenols

LaFeO₃/SiO₂ nanocomposite was synthesized by the sol–gel process from metal nitrates and tetraethyl orthosilicate (TEOS) as the SiO₂ source. The nanocomposite product was characterized by XRD, FT-IR, SEM, and surface area measurements and was used as a heterogeneous catalyst for the efficient acetylation of amines, alcohols and phenols to the corresponding acetates using acetic anhydride under solvent-free conditions. Among the various substrates, acetylation of amines was preceded rapidly, so that an amine group could be selectively acetylated in the presence of alcoholic or phenolic hydroxyl groups by the appropriate choice of reaction time. The catalyst can also be reused several times without the loss of activity. In addition, the catalytic activity of the LaFeO₃/SiO₂ nanocomposite was higher than that of the pure LaFeO₃ nanoparticles. The method is high yielding, clean, cost effective, compatible with the substrates having other functional groups and very suitable for the practical organic synthesis.