Efficient Solvent‐Free Synthesis of Benzothiazine‐Fused Pyrrolo[3,4‐c]coumarins: Cycloaddition Reactions between Coumarin‐Based Dihydrobenzothiazoles and Isocyanides

A new and unusual synthesis of benzothiazine‐fused pyrrolo[3,4‐c]coumarins, involving the ring‐opening of coumarin‐based dihydrobenzothiazoles and subsequent [4+1] cycloaddition reaction with isocyanides, was described. Thus, simple heating of various 3‐(2,3‐dihydro‐2‐methylbenzo[d]thiazol‐2‐yl)coumarins with isocyanides produced the title compounds in good yields under solvent‐free conditions.     

Synthesis and application of a thermosensitive tri-block copolymer as an efficient sample treatment technique for preconcentration and ultra-trace detection of lead ions

We have designed and synthesized a thermosensitive tri-block copolymer for selective trace extraction of Pb(II) ions from biological and food samples. The polymer was characterized by Fourier transform IR and NMR spectroscopy, and by gel permeation chromatography. The critical aggregation concentration and lower critical solution temperature were determined via fluorescence and UV spectrophotometry, respectively. The effects of solution pH value, amount of copolymer, of the temperature on extraction and on phase separation, and of the matrix on the extraction of Pb(II) were optimized. Pb(II) ions were then quantified by FAAS. The use of this copolymer resulted in excellent figures of merit including a calibration plot extending from 0.5 to 160 μg L^?1 (with an R² of >0.99), a limit of detection (LOD) as low as 90 pg L^?1, an extraction efficiency of >98 %, and relative standard deviations of <4 % for eight separate extraction experiments.

Screen-printed electrodes for biosensing: a review (2008–2013)

Screen-printing is one of the most promising approaches towards simple, rapid and inexpensive production of biosensors. Disposable biosensors based on screen printed electrodes (SPEs) including microelectrodes and modified electrodes have led to new possibilities in the detection and quantitation of biomolecules, pesticides, antigens, DNA, microorganisms and enzymes. SPE-based sensors are in tune with the growing need for performing rapid and accurate in-situ analyses and for the development of portable devices. This review (with 226 refs.) first gives an introduction into the topic and then is subdivided into sections (a) on DNA sensors (including methods for the detection of hybridization and damage), (b) on aptasensors (for thrombin, OTA, immunoglobulins and cancer biomarkers), (c) on immunosensors (for microorganisms, immunoglobulins, toxins, hormones, lactoferrin and biomarkers), (d) on enzymatic biosensors (for glucose, hydrogen peroxide, various pharmaceuticals, neurotransmitters, amino acids, NADH, enzyme based sensors).

Synthesis,Characterization and Photocatalytic Activity of Mg‐Impregnated ZnO–SnO2 Coupled Nanoparticles

ZnO–SnO₂ nanoparticles were prepared by coprecipitation method; then Mg, with different molar ratios and calcination temperatures, was loaded on the coupled nanoparticles by impregnation method. The synthesized nanoparticles were characterized by X‐ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X‐ray spectroscopy (EDX), transmission electron microscopy (TEM), diffuse reflectance spectroscopy (DRS), and Brunauer–Emmett–Teller (BET) techniques. Based on XRD results, the ZnO–SnO₂ and Mg/ZnO–SnO₂ nanoparticles were made of ZnO and SnO₂ nanocrystallites. According to DRS spectra, the band gap energy value of 3.13 and 3.18 eV were obtained for ZnO–SnO₂ and Mg/ZnO–SnO₂ nanoparticles, respectively. BET analysis revealed a Type III isotherm with a microporous structure and surface area of 32.051 and 49.065 m² g^?1 for ZnO–SnO₂ and Mg/ZnO–SnO₂, respectively. Also, the spherical shape of nanocrystallites was deduced from TEM and FESEM images. The photocatalytic performance of pure ZnO–SnO₂ and Mg/ZnO–SnO₂ was analyzed in the photocatalytic removal of methyl orange (MO). The results indicated that Mg/ZnO–SnO₂ exhibited superior photocatalytic activity to bare ZnO–SnO₂ photocatalyst due to high surface area, increased MO adsorption and larger band gap energy. Maximum photocatalytic activity of Mg/ZnO–SnO₂ nanoparticles was obtained with 0.8 mol% Mg and calcination temperature of 350°C.     

Novel Four-Step Synthesis of Thioxo-quinazolino[3,4-a]quinazolinone Derivatives

A novel synthesis of thioxo-quinazolino[3,4-a]quinazolinone framework was developed through a four-step reaction starting from isatoic anhydride. The resulting 2-aminobenzamides from the reaction of isatoic anhydride and different amines underwent coupling–cyclization reaction with 2-nitrobenzaldehydes, reduction of nitro group, and then cyclization reaction with carbon disulfide (CS₂). All steps were carried out under easy and user-friendly conditions in a short time without using expensive catalysts or reagents.

[Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the following free supplemental resource(s): Full experimental and spectral details.]     

Vilsmeier Reagent: An Efficient Reagent for the Transformation of 2-Aminobenzamides into Quinazolin-4(3H)-one Derivatives

Clean and easy preparation of quinazolin-4(3H)-one derivatives using 2-aminobenzamides and Vilsmeier reagent is described. 2-Aminobenzamides were converted into the corresponding quinazolinones under mild and efficient conditions, in good yields without undesirable by-products.

[Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the following free supplemental resource(s): Full experimental and spectral details.]     

Three component tandem reactions involving protected 2-amino indoles, disubstituted propargyl alcohols, and I2/ICl: iodo-reactant controlled synthesis of dihydro-α-carbolines and α-carbolines via iodo-cyclization/iodo-cycloelimination

Two simple, highly efficient three component tandem reactions for the synthesis of diversified N^aN^b di-carbamate-4,9-dihydro-3-iodo-α-carbolines and N^a-carbamate-3-iodo-α-carbolines have been described. The strategy involves one-pot condensation of bis-carbamate protected 2-amino indoles with disubstituted propargyl alcohols and I₂/ICl. The salient feature of the reaction involves iodocyclo-elimination of N^b-linked carbamate under mild condition in the final step.     

A facile synthesis of novel 1,4-benzoxazepin-2-one derivatives

An efficient and simple synthesis of 1,4-benzoxazepin-2-one derivatives has been achieved via the reaction of isoquinoline, activated acetylenes, and 1-(6-hydroxy-2-isopropenyl-1-benzofuran-yl)-1-ethanone in water without using any catalyst. This one-pot reaction occurs in high yields under mild conditions.     

An efficient one-pot method for the synthesis of novel ferrocene-triamide conjugates via pseudo five-component reaction

A simple and efficient one-pot synthesis of novel ferrocene-triamide conjugates from the reaction of ferrocenecarboxaldehyde with Meldrum’s acid and isocyanides in the presence of NH-containing compounds is described. This transformation proceeds through the creation of two CC bonds, two CN bonds, and one CO bond, leading to three peptide bonds, and presumably occurs via a domino sequence involving Knoevenagel condensation, [1+4] cycloaddition, deacetonation, and aminolysis reactions.