A novel synthesis of imidazo[1,2-a]quinoxalines

Several new derivatives of imidazo[1,2-a]quinoxalines have been synthesized in good to excellent yields starting from arylaminoisoxazol-5(2H)-ones and 2,3-dichloroquinoxaline through a rearrangement under mild base-catalyzed conditions.     

An Effective and New Method for the Synthesis of Polysubstituted Imidazoles by the Use of CrCl3.6H2O as a Green and Reusable Catalyst: Synthasis of Some Novel Imidazole Derivatives

New, efficient and environmentally adapted synthesis of polysubstituted imidazoles in one‐pot is found. The multicomponent reaction of various aldehydes, benzil, aliphatic and aromatic primary amines and ammonium acetate under solvent‐free condition is explained. The highly efficient role of CrCl₃.6H₂O as catalyst in this synthesis was shown. By this advantage, several polysubstituted imidazoles as pharmaceutical important molecules can be prepared in high yield and high purity. This method is a very easy and a rapid reaction for the synthesis of imidazole derivatives. The crude products recrystallized to afford the crystalline pure products. Furthermore, catalyst exhibited remarkable reusable activity.     

Rapid Synthesis of Novel and Known Coumarin‐3‐carboxylic Acids Using Stannous Chloride Dihydrate under Solvent‐Free Conditions

Various coumarin‐3‐carboxylic acid (=2‐oxo‐2H‐1‐benzopyran‐3‐carboxylic acid; CcaH) derivatives have been synthesized in good yields using catalytic amounts of SnCl₂?2 H₂O under solvent‐free conditions. This inexpensive, nontoxic, and readily available catalytic system (10 mol‐%) efficiently catalyzes the Knoevenagel condensation and intramolecular cyclization of various 2‐hydroxybenzaldehydes or acetophenones with Meldrum's acid. High product yields, use of inexpensive and safe catalyst, and solvent‐free conditions display both economic and environmental advantages.     

Two Novel Push?Pull Series of Benzothiazole‐Based Dyes: Synthesis and Characterization

New dichromophoric cyanine dyes based on benzothiazol‐2‐amines as push? pull systems were synthesized in two series of disperse and cationic forms (see 4 in Scheme 1 and 5 in Scheme 2, resp.). Their thermal stabilities, UV/VIS, fluorescence, and solvatochromic behavior, which are important parameters in push? pull systems, were also studied.     

Analysis of trace amounts of chlorobenzenes in water samples: An approach towards the automation of dynamic hollow fiber liquid-phase microextraction

We have combined dynamic hollow fiber liquid-phase microextraction with GC and electron capture detection for the quantitative determination of five chlorobenzenes in water samples. Extraction is based on an automated dynamic extraction device called TT-tube extractor which consists of a polypropylene hollow fiber mounted inside a stainless steel tube. Toluene is used as the extraction solvent that fills the lumen and pores of the hydrophobic fiber and flows through the lumen of the fiber using a programmable syringe pump. The type of organic solvent, ionic strength, diameter of the TT-tube, sample volume, and the times for extraction and dwelling were optimized. Under optimum conditions, the method gives limits of detection as low as 10–100?ng?L^?1, a linear dynamic range of 0.05–100?μg?L^?1, and relative standard deviations of <7% (n?=?6). The preconcentration factor can be as large as 562–973. In an example for a practical application, the chlorobenzenes were successfully determined in environmental aqueous samples. The hollow fiber membrane can be used at least 20 times without any carry-over or loss in extraction efficiency. The system is inexpensive and convenient, and requires minimal manual handling.

A simple and expedient method for the stepwise synthesis of 2-ethoxy-(4H)-3,1-benzoxazine-4-ones

A simple and practical route is described for the synthesis of 2-efhoxy-(4H)-3,1 -benzoxazine-4-ones using the coupling reaction of anthranilic acid derivatives with diethyl dicarbonate following with fast cyclization of the carbamate adduct with a dehydrocyclization agent such as cyanuric chloride and N,N′-dicyclohexylcarbodiimide in PEG at room temperature.High yields of the products obtained under mild reaction conditions with simple work-up of the reaction mixture.     

Ion-selective carbon paste electrode based on new tripodal ligand for determination of cadmium (II)

A new chemically modified carbon paste electrode for Cd(II) ions based on 3,5-dinitro-N-(tri-2-pyridyl methyl) benzamide (DNTPMBA) as an ionophore was prepared. The electrode exhibits a Nernstian response for Cd(II) ions over a wide concentration range (2.16 × 10^?7–1.00 × 10^?1 mol L^?1) with a slope of 30 ± 1 mV per decade. It has a response time of about 50 s and can be used for a period of 3 months with good reproducibility. Detection limit obtained in the optimal conditions was 1.82 × 10^?7 mol L^?1. The electrode was successfully used for potentiometric determination of Cd(II) in well water. The pH influence and interference of some cations were also studied.     

One-pot,three-component synthesis of polyfunctionalized benzo[h]pyrazolo[3,4-b][1,6]naphthyridine and benzo[g]pyrazolo[3,4-b]quinoline derivatives in the presence of silver nanoparticles (AgNPs)

An efficient and straightforward protocol for one-pot, three-component reaction of aryl glyoxal monohydrates 1a-h , 5-amino-1-aryl-3-methylpyrazoles 2a , b and 4-hydroxyquinoline-2(1H)-one ( 3 ) or 2-hydroxy-1,4-naphthoquinone ( 4 ) using silver nanoparticles (AgNPs) as a high performance nanocatalyst in H₂O/EtOH at 60°C afforded the corresponding polyfunctionalized benzo[h]pyrazolo[3,4-b][1,6]naphthyridines 5a-h and benzo[g]pyrazolo[3,4-b]quinolines 6a-i , respectively. Excellent catalytic activity, high yields, employing green media and green nanocatalyst, cost-effective and simple procedure are some notable advantages of using AgNPs as a noble metal nanocatalyst in this synthetic strategy. The structures of fused heterocycles were confirmed by their Fourier transform infrared, proton nuclear magnetic resonance (¹H-NMR), and ¹³C-NMR spectral data and microanalysis.     

Analysis of Paraben Preservatives in Cosmetic Samples: Comparison of Three Different Dynamic Hollow Fiber Liquid-Phase Microextraction Methods

This study focused on a comparison of three different dynamic hollow fiber-based liquid-phase microextraction (DHF-LPME) methods for extraction and preconcentration of parabens from wastewater, toothpaste, cream, and shampoo samples. The first method is two-phase DHF-LPME, in which n-octanol was used as the extraction solvent. The second is three-phase DHF-LPME, in which n-octanol and basic aqueous solution were used as the extraction solvent and acceptor phase, respectively. High-performance liquid chromatography with UV detection (HPLC–UV) was applied for determination of the parabens in both methods. The third method is a recently introduced method; three-phase DHF-LPME based on two immiscible organic solvents (n-dodecane as organic solvent and acetonitrile as an acceptor phase). The quantitative analyses were performed by the use of gas chromatography-mass spectrometry (GC–MS) after injection port derivatization. The effect of different extraction conditions (i.e., extraction solvent, pH, ionic strength, stirring rate, and dynamic and extraction times) on the extraction efficiency of the parabens was investigated and optimized. All the three procedures provide similar working parameters characterized by high repeatability (3.9–6.3 %) and good linearity (correlation coefficient ranging from 0.989 to 0.998). Results of real sample analyses obtained by these three methods were highly correlated. Although all methods provide compatible alternatives for paraben analysis, the three-phase DHF-LPME based on two immiscible organic solvents may be a more appropriate technique due to its higher extraction efficiency and thus lower limits of detection (LODs). LODs for all the parabens ranged from 0.2 to 5.0 μg L^?1 using the two first methods combined with HPLC–UV. An improvement in sensitivity of several orders of magnitude was achieved using three-phase DHF-LPME based on two immiscible organic solvents followed by single-ion monitoring GC–MS analyses (0.01–0.2 μg L^?1) due to compatibility of this technique with GC instrument.     

An efficient and facile regioselective synthesis of new substituted (E)-1-(3-aryl-7,8-dihydrocinnoline-5(6H)-ylidene)hydrazines and (1E,2E)-1,2-bis(3-aryl-7,8-dihydrocinnoline-5(6H)-ylidene)hydrazines

A study concerning the new substituted cinnoline synthesis is described. The use of a one-pot three-component method allows a simple regioselective and efficient synthesis of cinnoline derivatives via reaction of arylglyoxals with 1,3-cyclohexanedione and dimedone in the presence of hydrazine hydrate.