Microwave‐assisted Aqueous Multicomponent Reaction: Facile Synthesis of Polyfunctionalized Indoline‐spiro Fused Pyran Derivatives

A green and highly efficient method for the synthesis of polyfunctionalized indoline‐spiro fused pyran derivatives has been established. This reaction was conducted by reacting readily available and inexpensive starting materials, such as isatins, cyclic‐1,3‐dicarbonyl compounds, and malononitrile in aqueous media without any catalysts under microwave irradiation. The present green synthesis shows fascinating properties such as the use of water as the reaction solution, concise one‐pot conditions, short reaction periods (8–14 min), and easy purifications. The synthesis could also set a good example to GAP (Group‐Assistant‐Purification) chemistry in which purification via chromatography can be avoided and the pure products can be easily acquired only by washing the crude products with 95% EtOH.     

Facile synthesis of a porous network-like silver film for electrocatalytic detection of nitrate

We have developed a method for in-situ construction of a porous network-like silver film on the surface of a glassy carbon electrode (GCE). It is based on a galvanic replacement reaction where a layer of copper nanoparticles is first electrodeposited as a sacrificial template. The silver film formed possesses a porous network-like structure and consists of an assembly of numerous nanoparticles with an average size of 200 nm. The electrode displays excellent electrocatalytic activity, good stability, and fast response (within 2 s) toward the reduction of nitrate at a working potential of −0.9 V. The catalytic currents linearly increase with the nitrate concentrations in the range of 0.08–6.52 mM, with a detection limit of 3.5 μM (S/N = 3) and a repeatability of 3.4 % (n = 5).

A facile method was developed for in situ construction of a porous network-like Ag film on a glassy carbon electrode by a galvanic replacement reaction, where a layer of Cu nanoparticles previously electrodeposited as a sacrificial template. Thus-formed Ag film displays excellent electrocatalytic activity, good stability, and fast response (within 2 s) toward nitrate reduction.

     

A study on the direct electrochemistry and electrocatalysis of microperoxidase-11 immobilized on a porous network-like gold film: Sensing of hydrogen peroxide

We have prepared porous and network-like nanofilms of gold by galvanic replacement of a layer of copper particles acting as a template. The films were first characterized by scanning electron microscopy and X-ray diffraction, and then modified with cysteamine so to enable the covalent immobilization of the enzyme microperoxidase-11. The immobilized enzyme undergoes direct electron transfer to the underlying electrodes, and the electrode displays high electrocatalytic activity towards the reduction of oxygen and hydrogen peroxide, respectively, owing to the largely enhanced electroactive surface of the porous gold film. The detection limit of H₂O₂ is 0.4 μM (3 S/N).

Non-enzymatic hydrogen peroxide sensor based on a gold electrode modified with granular cuprous oxide nanowires

Granular nanowires with a diameter of about 60 nm were fabricated from cuprous oxide (Cu₂O) by an electrochemical method using anodic aluminium oxide as the template. A non-enzymatic sensor for hydrogen peroxide (H₂O₂) was then developed on the basis of a gold electrode modified with Cu₂O nanowires and Nafion. The resulting sensor enables the determination of H₂O₂ with a sensitivity of 745 μA?mM^?1?cm^?2, over a wide linear range (0.25 μM to 5.0 mM), and with a low detection limit (0.12 μM). The results demonstrate that the use of such granular nanowires provides a promising tool for the design of non-enzymatic chemical sensors.

Non-isothermal decomposition kinetics of diosgenin

The thermal stability and kinetics of isothermal decomposition of diosgenin were studied by thermogravimetry (TG) and Differential Scanning Calorimeter (DSC). The activation energy of the thermal decomposition process was determined from the analysis of TG curves by the methods of Flynn-Wall-Ozawa, Doyle, ?atava-?esták and Kissinger, respectively. The mechanism of thermal decomposition was determined to be Avrami-Erofeev equation (n = 1/3, n is the reaction order) with integral form G(α) = [?ln(1 ? α)]^1/3 (α = 0.10–0.80). E _a and logA [s^?1] were determined to be 44.10 kJ mol^?1 and 3.12, respectively. Moreover, the thermodynamics properties of ΔH ^≠, ΔS ^≠, and ΔG ^≠ of this reaction were 38.18 kJ mol^?1, ?199.76 J mol^?1 K^?1, and 164.36 kJ mol^?1 in the stage of thermal decomposition.     

An Efficient One-Pot Synthesis of Nitriles from Carboxylic Acids Without Solvent Under Microwave Irradiation

Nitriles were prepared from alkyl and aryl carboxylic acids in dry media conditions, under microwave irradiation. Heating of the carboxylic acid, urea and amidosulfonic acid adsorbed on alumina support in a microwave oven affords nitriles in 20–93% yields.     

Trans-2-Diethylphosphoryloxy-1,3-Pentadiene in The Lewis acid Catalyzed Diels-Alder Reaction

Under stannic chloride catalysis, trans-2-diethylphosphoryloxy-1,3-pentadiene (1) undergoes Diels-Alder reaction regio- and stereoselectively with a variety of α,β-unsaturated ketones at low temperature.     

Stereoselective Synthesis and Characterization of (Z)-(−)-4-(1′-Alkoxyl-1′-alkyloxycarbonyl-methylidene)-5(R)-[(1R)-menthyloxy]-γ-butyrolactones

Abstract

A series of enantiomerically pure (Z)-(?)-4-(1′-alkyloxy-1′-alkyloxycarbonyl-methylidene)-5(R)-[(1R)-menthyloxy]-γ-butyrolactones were synthesized and characterized in good to excellent yields via O-alkylation of (4R,5R)-(?)-4-ethoxyoxalyl-5-[(1R)-menthyloxy]-γ-butyrolactone with alkyl halides in the presence of K₂CO₃ in acetone at room temperature.     

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.      

Facile Synthesis of 5‐Benzylidene Rhodamine Derivatives under Microwave Irradiation

A series of 5‐benzylidenerhodamine derivatives were synthesized by the cross‐aldol condensation of an aromatic aldehyde with rhodamine or rhodamine acetic acid in sodium acetate/acetic acid under microwave irradiation. The reaction was completed in 8–20 min with 63–94% yields and was environmentally benign with easy workup.