Rapid and efficient synthesis of optically active pyrazoles under solvent-free conditions

2-Formyl glycals undergo rapid condensation with arylhydrazines under solvent-free conditions to give the corresponding optically pure 4-substituted pyrazoles in good yields with high selectivity. The stereochemistry of the products was assigned by various NMR experiments.     

Synthesis and antimicrobial activity of N-(substituted)-N'-(2,3-dihydro-2-oxido-5-benzoyl-1H-1,3,2-benzodiazaphosphol-2-yl) ureas

N-(substituted)-N'-(2,3-dihydro-5-benzoyl-2-oxido-1H-1,3,2-benzodiazaphosphol-2-yl) ureas were synthesized by reacting 3,4-diaminobenzophenone (4) with different chlorides of carbamidophosphoric acids (3) in the presence of triethylamine at 40-45 degrees C. Their 1H-, 13C- and 31P-NMR spectral data are discussed. The title compounds were screened for antifungal and antibacterial activity against the fungi Aspergillus niger and Fusarium solani and bacteria Escherichia coli and Staphylococcus aureus. These compounds showed higher antibacterial activity when compared with antifungal activity.     

Donor properties of some flexidentate hydroxyimino-β-diketones in their rhodium(III) complexes

Summary A series of rhodium(III) complexes of certain hydroxyimino--diketones were synthesised and their structures assigned on the basis of elemental analyses and i.r. and¹H n.m.r. spectral studies, The complexes exhibit coordination through carbonyl oxygen and nitrogen of the hydroxy-imino groups in the ligands.¹H and¹³C n.m.r. studies show that the ligands exist in the isonitroso form in CDCl₃.     

Third‐order WENO scheme with a new smoothness indicator

In this article, we have devised a new reference smoothness indicator for third‐order weighted essentially non‐oscillatory (WENO) scheme to achieve desired order of convergence at critical points. In the context of the weighted essentially non‐oscillatory scheme, reference smoothness indicator is constructed in such a way that it satisfies the sufficient condition on the weights for the third‐order convergence. The goal is to construct a reference smoothness indicator such that the resulted scheme have to achieve the required order of accuracy even if the first two derivatives vanish but not the third derivative. The construction of such reference smoothness indicator is not possible through a linear combination of local smoothness indicators only. We have proposed a reference smoothness indicator to be of the fourth order of accuracy on three‐point stencil that contains the linear combination of the first derivative information of the local and global stencils. The performance enhancement of the WENO scheme through this reference smoothness indicator is verified through the standard numerical experiments. Numerical results indicate that the new scheme provides better results in comparison with the earlier third‐order WENO schemes like WENO‐JS and WENO‐Z. Copyright © 2017 John Wiley & Sons, Ltd.     

Urea and thiourea derivatives of 3-(trifluoromethyl)-5,6,7,8-tetrahydro-[1, 2, 4]triazolo[4,3-a]pyrazine: Synthesis,characterization, antimicrobial activity and docking studies

Abstract

An efficient and robust synthetic procedure was developed primarily for the synthesis of a precursor compound; 3-(trifluoromethyl)-5,6,7,8-tetrahydro-[1, 2, 4]triazolo[4,3-a]pyrazine (11), from 2-chloropyrazine (7) through the chemical transformations such as hydrazine substitution, trifluoroacetyl group induction, cyclization and pyrazine ring reduction. A new series of urea derivatives 13a-e and thiourea derivatives 13f-j of compound 11 have been synthesized and the structures of all the compounds were confirmed using spectroscopic analyses such as IR, ¹H NMR, ¹³C NMR, LC-MS and HRMS. The newly synthesized compounds were screened for their in vitro antimicrobial activity against five bacteria and two fungi, in which compounds 13d, 13i and 13j displayed potential activity against bacterial strains and 13a, 13d, 13g and 13j against fungal strains with the MIC values in the range of 6.25–25.0 µg/mL. An overall comparison of the activity results revealed that thiourea derivatives contain better activity than that of urea compounds. Molecular docking studies on poly (ADP-ribose) polymerase 15 (ARTD7, BAL3) demonstrated that all the synthesized compounds possess significant binding energies (-8.1 to -9.8?kcal/mol) with no adverse effect in the active site of protein.     

Synthesis of New Benzoxazaphosphinine/Benzoxazaphosphole/Diazaphosphaphenalene‐2‐sulfides using Lawesson's Reagent

Synthesis of new benzoxazaphosphinine/benzoxazaphosphole/diazaphosphaphenalene 2‐sulfides were accomplished by the reaction of Lawesson's reagent (LR) with 4‐bromo‐2‐[(phenylamino) methyl]phenol (1a), 4‐bromo‐2‐[(4‐chloro/bromo/methoxy/methylphenyl‐amino)methyl]phenol (1b–e), 4‐bromo‐2‐[(benzylamino)methyl]phenol (1f), 2‐amino‐4‐chlorophenol (2a)/2‐amino‐4‐methylphenol (2b), 1,8‐diaminonaphthalene (3) respectively in anhydrous toluene. Products 4a–f, 5a–b and 6 were characterized by IR, ¹H, ¹³C, ³¹P NMR and Mass spectra.     

Synthesis and Antimicrobial Activity of 1‐[(Substituted Carbamoyl)Amino]‐1H,3H‐1λ5‐[1,3,2]oxazaphospholo[3,4‐a]benzimidazol‐1‐ones

1‐[(Substituted carbamoyl)amino]‐1H,3H‐1λ⁵‐[1,3,2]oxazaphospholo[3,4‐a]benzimidazol‐1‐ones were synthesized by reacting benzimidazole 2‐methanol (4) with different chlorides of carbamidophosphoric acids (3) in the presence of triethylamine at 40–45°C. Their ¹H, ¹³C, and ³¹P NMR spectral data were discussed. The title compounds were tested for their activity against the fungi Aspergillus niger and Fusarium solani and bacteria Staphylococcus aureus and Escherichia coli. These compounds showed moderate antibacterial activity when compared with antifungal activity.     

Silk‐Pectin Hydrogel with Superior Mechanical Properties,Biodegradability, and Biocompatibility

A new method is developed to prepare silk hydrogels and silk‐pectin hydrogels via dialysis against methanol to obtain hydrogels with high concentrations of silk fibroin. The relationship between the mechanical and biological properties and the structure of the silk‐pectin hydrogels is subsequently evaluated. The present results suggest that pectin associates with silk molecules when the silk concentration exceeds 15 wt%, suggesting that a silk concentration of over 15 wt% is critical to construct interacting silk‐pectin networks. The silk‐pectin hydrogel reported here is composed of a heterogeneous network, which is different from fiber‐reinforced, interpenetrated networks and double‐network hydrogels, as well as high‐stiffness hydrogels (elastic modulus of 4.7 ± 0.9 MPa, elastic stress limit of 3.9 ± 0.1 MPa, and elastic strain limit of 48.4 ± 0.5%) with regard to biocompatibility and biodegradability.     

Thermal performance of stable SiO2 nanofluids and regression correlations to estimate their thermophysical properties

The present work investigates the best mix ratio of Glycerol in Water as a medium to prepare a stable nanofluid. Increasing the proportion of glycerol enhances the aqueous mix's dynamic viscosity and improves the prepared nanofluid's stability. The thermal conductivity and viscosity of the Glycerol and Water mixtures determination were undertaken at various Glycerol ratios. The best percentage of glycerol in the mixture is found to have the least amount of thermal conductivity loss and the optimum viscosity gain. Silica (SiO₂) nanofluid of 0.25%, 0.5%, 1%, and 1.5% weight concentrations was prepared with this optimal mixture of Glycerol and Water. The stability of these SiO₂ nanofluids is evaluated by determining the zeta potential at different time intervals. The nanofluids prepared were observed to be stable for one month. The thermal conductivity and viscosity of the nanofluids are measured between the temperature limits of 30°–70°C. A peak increment of 32.1%and 46.3% in thermal conductivity and viscosity is observed. Furthermore, when the percentage enhancement ratio (PER) and Mouromtseff ratio of these nanofluids is examined, it is observed that they have more excellent thermal performance at higher temperatures. Regression correlations are developed to estimate the thermal conductivity and viscosity of the prepared nanofluids with a maximum deviation of 9%.