A facile microwave assisted synthesis of spiro-1,3-oxazines from N-(2-(cyclohex-1-en-1-yl)ethyl)amides

A mild and efficient methodology has been developed for the synthesis of spiro-1,3-oxazine derivatives by the microwave assisted cyclization of N-2-(1′-cyclohexenyl)ethyl-acetamides/benzamides. The reaction was catalyzed by in situ generated trimethylsilyl iodide and featured by its very short reaction time. The starting materials were easily obtained by the condensation of substituted acetic/benzoic acids with 2-(1′-cyclohexenyl)ethyl amine.     

A novel microwave-mediated one-pot synthesis of indolizines via a three-component reaction

[reaction: see text] The microwave-mediated three-component reaction of acyl bromide, pyridine, and acetylene is catalyzed by basic alumina to give corresponding indolizines in excellent yields in a one-pot reaction.     

Influence of Sn on the hydration of tricalcium aluminate, Ca3Al2O6

Tricalcium aluminate (Ca₃Al₂O₆, C₃A) containing 0?C5% of Sn was synthesized by solid-state method, and the products were characterized by XRD technique. Differential thermo-analytical technique (DTA) along with X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM) were applied to study the hydration behaviour of different C₃A samples with and without the presence of gypsum. Results indicate that C₃A can accommodate small amount of Sn in its structure and remaining amount forms SnO₂. Hydration studies of the synthesized C₃A shows that the additions of 0.5 and 1% Sn increase and 2% Sn decrease the reactivity of C₃A at the initial period (<3?h) of hydration. Increasing additions of Sn also increase the amounts of amorphous phases and hexagonal calcium aluminate hydrates in the cement pastes. The stabilities of these hydration products also increase with increasing content of Sn in C₃A at the experimental conditions. The presence of Sn significantly changes the hydration of C₃A and gypsum solid mixture at the initial period of hydration by enhancing the formation of more amounts of AFt and AFm phases. However, at the later stage of hydration (on or after 3?days), the hydration products in C₃A and gypsum pastes with and without the presence of Sn are almost similar.     

Chemistry of trichlorofluoromethane: synthesis of chlorofluoromethyl phenyl sulfone and fluoromethyl phenyl sulfone and some of their reactions.

It was observed that the reaction of CFCl3 with thiophenoxide gave only 10% of the corresponding thioether. On the other hand, these thioethers could be prepared in excellent yield from diaryl disulfides and CFCl3 in the presence of sodium hydroxymethanesulfinate in aqueous DMF at 4 atm pressure of nitrogen. Dechlorination of the thioether (PhSCFCl2) with different reducing agents were studied. Most of the reducing agents eliminated both fluorine and chlorine functionalities or gave the hydrolyzed products. But its sulfone on treatment with Zinc in methanol gave monochlorofluoromethyl and fluoromethyl phenyl sulfone in good yields. Darzens reaction of these compounds was also studied.     

Motional dispersions and ratchet effect in inertial systems

We obtain ratchet effect in inertial structureless systems in symmetric periodic potentials where the asymmetry comes from the non-uniform friction offered by the medium and driven by symmetric periodic forces. In the adiabatic limit the calculations are done by extending the matrix continued fraction method and also by numerically solving the appropriate Langevin equation. For finite frequency field drive the ratchet effect is obtained only numerically. In the transient time scales the system shows dispersionless behaviour as reported earlier when a constant force is applied. In the periodic drive case the dispersion behaviour is more complex. In this brief communication we report some of the results of our work.      

Dehydration kinetics of an Indian clay

Decomposition of clay from Garo Hills of Meghalaya (India) was studied by dynamic thermogravimetry. A fourteen kinetic equation procedure was applied for analysis of non-isothermal weight change upto a temperature of 1223 K. Two stages of decomposition were clearly distinguised i.e. the initial dehydration period at temperature 373 K to 673 K and the dehydroxylation period in the temperature range 723 K to 1073 K. First order decomposition mechanism was found to be applicable to both dehydration and dehydroxylation steps. Activation energies of 67 kJ/mol and 278 kJ/mol are estimated for the first and second steps with frequency factors of 16.3 s^–1 and 5.16×10⁶s^–1 respectively. The weight loss relating to the steps in TG curves allows determination of the contents of the basic mineral in the clay. Percentages of Al₂O₃.SiO₂ and total volatiles as calculated from weight loss data are in accordance with the results of classical chemical analysis.

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Zusammenfassung Mittels DTG wurde die thermische Zersetung von Ton aus der Garo-Hills-Gegend bei Meghalaya (Indien) untersucht. Zur Analyse der nicht-isothermen Gewichtsveränderungen bis zu einer Temperatur von 1223 K wurde ein Verfahren mit vierzehn kinetischen Gleichungen angewendet. Zwei Teilschritte der Zersetzung können eindeutig unterschieden werden, nämlich die anfängliche Dehydratationsperiode bei Temperaturen von 373 bis 673 K und die Dehydroxylierungsperiode bei Temperaturen zwischen 723 K un 1073 K. Für beide Vorgänge konnte als Reaktionsmechanismus eine Zersetzung erster Ordnung angewendet werden. Für den ersten un zweiten Teilschritt konnten Aktivierungsenergien von 67 kJ/mol bzw. 278 kJ/mol un Frequenzfaktoren von 16.3s^–1 bzw. 5.16×10⁶s^–1 ermittelt werden. Der aus den TG-Kurven hervorgehende Gewichtsverlust läßt auf den Gehalt des Tones an Basismineral schließen. Der prozentuelle Gehalt an Al₂O₃, SiO₂ und der gesamten flüchtigen Bestandteile, berechnet aus den Gewichtsverlusdaten, stimmt mit den Ergebnissen aus herkömmlichen chemischen Analysen überein.

     

Some new proofs of modular relations for the Göllnitz-Gordon functions

In this paper, we find new proofs of modular relations for the Göllnitz-Gordon functions established earlier by S.-S. Huang and S.-L. Chen. We use Schröter’s formulas and some simple theta-function identities of Ramanujan to establish the relations. We also find some new modular relations of the same nature.     

Banana pulp extract mediated synthesis of Cu2O nanoparticles: An efficient heterogeneous catalyst for the ipso-hydroxylation of arylboronic acids

A green and facile novel procedure has been developed for the synthesis of Cu₂O nanoparticles within a very short reaction time using banana pulp extract as a reducing agent. The synthesized nanoparticles are well characterized by SEM (Scanning Electron Microscope), TEM (Transmission Electron Microscope) and powder XRD (X-ray Diffraction) methods. An environmental benign and highly efficient protocol for the ipso-hydroxylation of aryl and hetero arylboronic acids using bio-fabricated Cu₂O nanoparticles as a catalyst and aqueous H₂O₂ as an oxidant has also been developed. The main advantages of this protocol are the base free reaction condition, reusable and heterogeneous catalytic system, and short reaction time with excellent yields.     

Optical and dielectric properties of isothermally crystallized nano-KNbO3 in Er3+-doped K2O–Nb2O5–SiO2 glasses

Precursor glass of composition 25K₂O–25Nb₂O₅–50SiO₂ (mol%) doped with Er₂O₃ (0.5 wt% in excess) was isothermally crystallized at 800 °C for 0–100 h to obtain transparent KNbO₃ nanostructured glass–ceramics. XRD, FESEM, TEM, FTIRRS, dielectric constant, refractive index, absorption and fluorescence measurements were carried out to analyze the morphology, dielectric, structure and optical properties of the glass–ceramics. The crystallite size of KNbO₃ estimated from XRD and TEM is found to vary in the range 7–23 nm. A steep rise in the dielectric constant of glass–ceramics with heat-treatment time reveals the formation of ferroelectric nanocrystalline KNbO₃ phase. The measured visible photoluminescence spectra have exhibited green emission transitions of ²H_11/2, ⁴S_3/2 → ⁴I_15/2 upon excitation at 377 nm (⁴I_15/2 → ⁴G_11/2) absorption band of Er³⁺ ions. The near infrared (NIR) emission transition ⁴I_13/2 → ⁴I_15/2 is detected around 1550 nm on excitation at 980 nm (⁴I_15/2 → ⁴I_11/2) of absorption bands of Er³⁺ ions. It is observed that photoluminescent intensity at 526 nm (²H_11/2 → ⁴I_15/2), 550 nm (⁴S_3/2 → ⁴I_15/2) and 1550 nm (⁴I_13/2 → ⁴I_15/2) initially decrease and then gradually increase with increase in heat-treatment time. The measured lifetime (τ_f) of the ⁴I_13/2 → ⁴I_15/2 transition also possesses a similar trend. The measured absorption and fluorescence spectra reveal that the Er³⁺ ions gradually enter into the KNbO₃ nanocrystals.     

Structural, optical and electrical properties of tin oxide thin film deposited by APCVD method

Tin oxide (SnO₂) thin films have been grown on glass substrates using atmospheric pressure chemical vapour deposition (APCVD) method. During the deposition, the substrate temperature was kept at 400°C–500°C. The structural properties, surface morphology and chemical composition of the deposited film were studied by X-ray diffraction (XRD), scanning electron microscope (SEM) and Rutherford back scattering (RBS) spectrum. XRD pattern showed that the preferred orientation was (110) having tetragonal structure. The optical properties of the films were studied by measuring the transmittance, absorbance and reflectance spectra between λ = 254 nm to 1400 nm and the optical constants were calculated. Typical SnO₂ film transmits ∼ 94% of visible light. The electrical properties of the films were studied using four-probe method and Hall-voltage measurement experiment. The films showed room temperature conductivity in the range 1.08 × 10² to 1.69 × 10² Ω⁻¹cm⁻¹.