Electroless Ni–P coated on graphite as catalyst for the electro-oxidation of dextrose in alkali solution

Graphite particles were coated with Ni–P by electroless deposition using a conventional bath consisting of a nickel salt and hypophosphite. After 15 min of electroless deposition, the graphite particles were covered with 10 wt% nickel and 0.7–1.0 wt% phosphorus as analysed by wet chemical method. Surface morphology was studied by scanning electron microscopy (SEM). Electrochemical characterisation for the catalytic activity was done by cyclic voltammetry. Pure Ni powder and electroless Ni–P coated on graphite were used as catalysts for the electro-oxidation of dextrose (1.8 × 10⁻³ to 4.5 × 10⁻³ M) in 0.1 M KOH solution. Comparative studies revealed that electroless Ni–P coated on graphite particles acted as a better catalyst than pure Ni powder for catalytic reaction.     

Thermodynamic functions for U0.45Pu0.55N

Enthalpy increments of U_0.45Pu_0.55N were measured in the temperature range of 1025–1775 K by inverse drop calorimetry using a high temperature differential calorimeter. The enthalpy increments were fitted to a polynomial in temperature and the heat capacity, entropy and Gibbs energy functions were computed. The results are presented and discussed in comparison with literature data.     

Tandem versus single C-C bond forming reaction under palladium-copper catalysis: regioselective synthesis of α-pyrones fused with thiophene

We herein report a highly convenient protocol for rapid construction of α-pyrone fused with thiophene. This includes one-pot and regioselective synthesis of 4,5-disubstituted and 5-substituted thieno[2,3-c]pyran-7-ones, 6,7-disubstituted and 6-substituted thieno[3,2-c]pyran-4-ones. The synthesis of thieno[2,3-c]pyran-7-ones involves palladium mediated cross coupling of 3-iodothiophene-2-carboxylic acid with terminal alkynes in a simple synthetic operation. The coupling-cyclization reaction was initially studied in the presence of Pd(PPh₃)₂Cl₂ and CuI in a variety of solvents. 5-Substituted 4-alkynylthieno[2,3-c]pyran-7-ones were isolated in good yields when the reaction was performed in DMF. Similarly, 6-substituted 7-alkynylthieno[3,2-c]pyran-4-ones were synthesized via palladium-catalyzed cross coupling of 2-bromothiophene-3-carboxylic acid with terminal alkynes. A tandem C-C bond forming reaction in the presence of palladium catalyst rationalizes the formation of coupled product in this apparently three-component reaction. The cyclization step of this coupling-cyclization-coupling process occurs in a regioselective fashion to furnish products containing six-membered ring only. This sequential C-C bond forming reaction however, can be restricted to the formation of single C-C bond by using 10% Pd/C-Et₃N-CuI-PPh₃ as catalyst system in the cross coupling reaction. 5-Substituted thieno[2,3-c]pyran-7-ones were obtained in good yields when the coupling reaction was performed under this condition. Some of the compounds synthesized were tested in vitro for their anticancer activities.     

Bis(4,5-dimethoxy-2-nitrophenyl)ethylene glycol: a new and efficient photolabile protecting group for aldehydes and ketones

Synthesis of a new photolabile protecting group, bis(4,5-dimethoxy-2-nitrophenyl)ethylene glycol (4) from 4,5-dimethoxy-2-nitrobenzyl alcohol in three steps in good yields is described. The acetals and ketals of 4 are stable against acidic and basic reaction conditions and are cleaved smoothly on irradiation at 350 and 400 nm with regeneration of carbonyl compounds in high yields and efficiency.     

The Novel Formation of Ordered and Varied Silica-Imidazole Complexes from Silicic Acid

Abstract

Fixed quantities of silicic acid in isopropyl alcohol were treated with varying amounts of imidazole in the same solvent, left closed till complexation was complete (～7 days) and the resulting gels on slow evaporation (～30 days) afforded glassy solids, ranging from nodules to tubules, as seen by scanning electron microscope (SEM). In another strategy where soluble oligomers of silica along with monomers can be present and the reaction conditions remaining the same, rectangular cubes of varying sizes were secured. In the view of the significance and potential utility of this novel finding, only duplicate runs, which essentially afforded similar SEM are included here. Elemental analysis established the presence of imidazole in the complexes and their percentage composition was computed using thermo gravimetric analysis (TGA). FTIR showed organics, presence of hydrogen-bonded imidazole, Si?O?Si bonds, and complete absence of Si?O?C bonds. It is suggested that a pattern where hydrogen-bonded imidazole with itself and the polymer, is entombed in the polymerized silicic acid. Domains having such a profile most likely lead to the observed morphology.The present work vastly widens the scope for silicic acid—guest complexation and holds potential to discover a range of silica harboring materials.

GRAPHICAL ABSTRACT      

Synthesis of Novel (3a,S)‐1‐Aryl/aryloxy/alkoxy‐3a,4‐dihydro‐3H‐1λ5‐[1,3,2]oxazaphospholo [3,4‐a] indole‐1‐ones,Thiones, and Selenones

Synthesis of novel (3a,S)‐1‐aryl/aryloxy/alkoxy‐3a,4‐dihydro‐3H‐1λ⁵‐[1,3,2]oxazaphospholo [3,4‐a] indole‐1‐ones, thiones, and selenones was achieved in two steps with high yields from 2,3‐dihydro‐1H‐indol‐2(S)yl methanol (1) and dichlorophenyl phosphine/ethyl dichlorophosphite (2a and b) in the presence of triethylamine in dry THF followed by treatment with hydrogen peroxide, sulfur, and selenium. The compounds 4g–k have been synthesized by the direct cyclocondensation of 1 with different substituted phenyl phosphorodichloridates (2c–e, g) and bis(2‐chloroethyl) phosphoramidic dichloride (2f).     

Synthesis,biological evaluation and molecular docking studies of novel 2-(2-cyanophenyl)-N-phenylacetamide derivatives

A series of novel 2-(2-cyanophenyl)-N-phenylacetamide derivatives 3(a-u) were designed and synthesized via selective amidation of methyl-2-(2-cyanophenyl)acetates over amidine formation by using AlMe₃ as catalyst in good yields. All the newly synthesized derivatives were well characterized by ¹H NMR, ¹³C NMR, FTIR and HRMS spectral techniques. All the synthesized title compounds were evaluated for their in vitro anticancer activity against three cancer cell lines. Among all compounds, 3i (IC₅₀?=?1.20 μM, IC₅₀?=?1.10 μM), 3j (IC₅₀?=?0.11 μM, IC₅₀?=?0.18 μM), 3o (IC₅₀?=?0.98 μM, IC₅₀?=?2.76 μM) showed excellent inhibitory activity than the standard Etoposide (IC₅₀?=?2.11 μM, IC₅₀?=?3.08 μM) against MCF-7 and A-549 cell lines, respectively. Docking analysis of all the compounds with the human topoisomerase II revealed that the compound 3j fitted well in the active site pocket, showing the best docking score of 158.072 kcal/mol.

     

Measurement of line intensities of linear molecules under low resolution

By using the relation k_v?S_J/δ_J applicable at sufficiently high pressures, at which the rotational fine structure in a band is smeared out completely, line intensities S_J may be determined from measured spectral absorption coefficients and known local line spacings δ_J. First, the validity of the approximation is ascertained by comparing the spectral absorption coefficient data of Penner and Weber and of Varanasi and Penner for the fundamental bands of CO and NO, respectively, with S_J/δ_J derived from the high resolution measurements of Benedict et al. (for CO) and of Abels and Shaw (for NO). Line intensity data obtained using this method are in good agreement with the high-resolution measurements of Toth (grating spectroscopy) for some unblended lines in the 00°0?02°1 band of N₂O and of Lacome et al. (laser- spectroscopy) for lines in the 10°0?00°1 band of N₂O.     

Fluorescence characteristics of Dy ions in calcium fluoroborate glasses

Calcium fluoroborate (CFB) glasses doped with different concentrations of trivalent dysprosium ions were prepared and investigated by the FTIR, optical absorption, photoluminescence and decay analysis. Free-ion Hamiltonian model and Judd-Ofelt theory have been used to analyze the energy level scheme and the spectral intensities of Dy³⁺ ions in CFB glasses. From the emission spectra it is observed that the samples emit intense light yellowish color which is nearer to white light. Chromaticity color coordinates have been calculated and the dominant emission wavelength has also been indicated. Decay curves of ⁴F_9/2 level for the samples with different concentrations have been analyzed using the Inokuti-Hirayama model and the energy transfer and non-radiative decay rates have been determined.     

Observation of nanostripes and -clusters in (Nd, EuGd)Ba2Cu3Ox superconductors

Nanostripes are observed in melt-textured and single-crystalline samples of the ternary light rare earth (LRE)-compound (Nd_0.33Eu_0.33Gd_0.33)Ba₂Cu₃O_x (NEG) by means of atomic force microscopy, scanning tunnelling microscopy at ambient conditions, combined with transmission electron microscopy and electron backscatter diffraction. This enables the observation of several important features: The nanostripes are formed by chains of nanoclusters, representing the LRE/Ba substitution. The dimensions of the nanostripes are similar for both types of NEG samples. The periodicity of the nanostripes is found to range between 40 and 60 nm; the shape of the nanoclusters is elliptic with a major axis length between 300 and 500 nm and a minor axis length of about 30–150 nm. The stripes are filling effectively the space in between the twin boundaries. Concerning the flux pinning, the nanoclusters are the important pinning sites, not the nanostripes themselves.