An unusual, mild and convenient one-pot two-step access to (E)-stilbenes from hydroxy-substituted benzaldehydes and phenylacetic acids under microwave activation: a new facet of the classical Perkin reaction

A mild and convenient one-pot two-step synthesis of hydroxystilbenes with trans selectivity has been developed through a modified Perkin reaction between benzaldehydes and phenylacetic acids bearing 4- or 2-hydroxy substitution at the aromatic ring, in the presence of piperidine-methylimidazole and polyethylene glycol under microwave irradiation. The observation of a simultaneous condensation-decarboxylation leading to the unusual formation of hydroxystilbenes in lieu of α-phenylcinnamic acid reveals an interesting facet to the classical Perkin reaction. The developed protocol provides a green alternative to the prevalent methods employing a toxic decarboxylating agent in the form of quinoline/Cu salt, and the requirement for harsh protection-deprotection steps for the synthesis of hydroxylated stilbenes.     

Alkali Metal and Alkaline Earth Metal Complexes with the Bis(borane‐diphenylphosphanyl)amido Ligand – Synthesis,Structures, and Catalysis for Ring‐Opening Polymerization of ϵ‐Caprolactone

The syntheses of lithium and alkaline earth metal complexes with the bis(borane‐diphenylphosphanyl)amido ligand ( 1 ‐ H ) of molecular formulas [{κ²‐N(PPh₂(BH₃))₂}Li(THF)₂] ( 2 ) and [{κ³‐N(PPh₂(BH₃))₂}₂M(THF)₂] [(M = Ca ( 3 ), Sr ( 4 ), Ba ( 5 )] are reported. The lithium complex 2 was obtained by treatment of bis(borane‐diphenylphosphanyl)amine ( 1 ‐ H ) with lithium bis(trimethylsilyl)amide in a 1:1 molar ratio via the silylamine elimination method. The corresponding homoleptic alkaline earth metal complexes 3 – 5 were prepared by two synthetic routes – first, the treatment of metal bis(trimethylsilyl)amide and protio ligand 1 ‐ H via the elimination of silylamine, and second, through salt metathesis reaction involving respective metal diiodides and lithium salt 2 . The molecular structures of lithium complex 2 and barium complex 5 were established by single‐crystal X‐ray diffraction analysis. In the solid‐state structure of 2 , the lithium ion is ligated by amido nitrogen atoms and hydrogen atoms of the BH₃ group in κ²‐coordination of the ligand 1 resulting in a distorted tetrahedral geometry around the lithium ion. However, in complex 5 , κ³‐coordination of the ligand 1 was observed, and the barium ion adopted a distorted octahedral arrangement. The metal complex 5 was tested as catalyst for the ring opening polymerization of ?‐caprolactone. High activity for the barium complex 5 towards ring opening polymerization (ROP) of ?‐caprolactone with a narrow polydispersity index was observed. Additionally, first‐principle calculations to investigate the structure and coordination properties of alkaline earth metal complexes 3 – 5 as a comparative study between the experimental and theoretical findings were described.     

Validated Chiral LC Method for the Enantiomeric Separation of β-Amino-β-(3-Methoxyphenyl) Propionic Acid

A chiral liquid chromatographic method for enantiomeric resolution of β-amino-β-(3-methoxyphenyl) propionic acid was developed and validated. The “hybrid” π-electron donor–acceptor based stationary phase (R,R) Whelk-01 was found to be enantiomerically selective for (R) and (S) enantiomers of β-amino-β-(3-methoxyphenyl) propionic acid with a resolution greater than 2.0. The effects of isopropyl alcohol and ethanol on enantioselectivity and resolution of enantiomers were evaluated. Calibration curves were linear over the range of 0.10–1.00, with a regression coefficient (r) of 0.999. The limit of detection (LOD) and limit of quantification (LOQ) were 300 and 1,000 ng mL⁻¹ respectively for 10 μL injection volume. The percentage RSD of the peak area of six replicate injections of (S) enantiomer at LOQ concentration was 2.8. The percentage recovery of (S) enantiomer from (R) enantiomer samples ranged from 92 to 102. The test solution was observed to be stable up to 24 h after the preparation. The developed normal phase chiral LC method can be used for the enantiomeric purity evaluation of R-β-amino-β-(3-methoxyphenyl) propionic acid.     

Development of 99Mo-alfa-benzoin oxime complex as industrial radiotracer for identification of leaky heat exchanger and its validation with 99mTc

Journal of Radioanalytical and Nuclear Chemistry - In the traditional medicine of Iran, some herbal medicines are used for treating of high blood sugar. In this study, the concentration of Ca, Cr,...     

Role of micro-crystalline parameters in the physical properties of cotton fibers

Karnataka state in India is very well known for its cotton cultivation and there are innumerable varieties of these cotton fibers. Although, the yield and other types of characterization have been carried out on these fibers, the structure-property relation is not well studied till today. We have examined four different raw cotton fibers using Wide Angle X-ray Scattering (WAXS) technique and also we have computed micro-crystalline parameters. This study brings out the structure-property relation in cotton fibers.     

Langmuir-Blodgett films of 9-phenyl anthracene molecules incorporated into different matrices

This communication reports the surface pressure (pi) versus area per molecule (A) isotherm characteristics of the mixed films of 9-phenyl anthracene (PA) in stearic acid (SA) and polymethyl methacrylate (PMMA) matrices, at the air-water interface. The mixed Langmuir films at the air-water interface have been observed to be easily transferred onto solid substrates to form uniform Langmuir-Blodgett films. By changing various parameters, namely molefraction, surface pressure of lifting and number of layers, the mixed Langmuir-Blodgett (LB) films of various types have been fabricated successfully and their spectroscopic characteristics have been reported. From the isotherm characteristics and the area per molecule versus molefraction plot, it is evident that the PA molecules are successfully incorporated into mixed Langmuir-Blodgett films. UV-vis absorption spectroscopic study of the mixed LB films at various molefractions of PA in two different matrices reveal that formation of I-type aggregate in PMMA matrix whereas both I- and H-type aggregates are playing their dominant role in SA matrix. Moreover, fluorescence spectroscopic study reveals reabsorption effect. Molecular movement persists in the freshly prepared LB films, as is evident from the time dependent changes in both UV-vis absorption and fluorescence spectra of the mixed LB films in both matrices. From our observation it is evident that about 200 h is required to get the LB films in a stable condition. Dimers and higher order n-mers are formed at a higher surface pressure of 30 mNm(-1).     

Transient streaming potential in a finite length microchannel

Pressure-driven flow of an electrolyte solution in a microchannel with charged solid surfaces induces a streaming potential across the microchannel. Such a flow also causes rejection of ions by the microchannel, leading to different concentrations in the feed and permeate reservoirs connecting the capillary, which forms the basis of membrane based separation of electrolytes. Modeling approaches traditionally employed to assess the streaming potential development and ion rejection by capillaries often present a confusing picture of the governing electrochemical transport processes. In this paper, a transient numerical simulation of electrochemical transport process leading to the development of a streaming potential across a finite length circular cylindrical microchannel connecting two infinite reservoirs is presented. The solution based on finite element analysis shows the transient development of ionic concentrations, electric fields, and the streaming potential over the length of the microchannel. The transient analysis presented here resolves several contradictions between the two types of modeling approaches employed in assessing streaming potential development and ion rejection. The simulation results show that the streaming potential across the channel is predominantly set up at the timescale of the developing convective transport, while the equilibrium ion concentrations are developed over a considerably longer duration.     

Conditional VaR estimation using Pearson’s type IV distribution

This paper presents a new value at risk (VaR) estimation model for equity returns time series and tests it extensively on Stock Indices of 14 countries. Two most important stylized facts of such series are volatility clustering, and non-normality as a result of fat tails of the return distribution. While volatility clustering has been extensively studied using the GARCH model and its various extensions, the phenomenon of non-normality has not been comprehensively explored, at least in the context of VaR estimation. A combination of extreme value theory (EVT) and GARCH has been explored to analyze financial data showing non-normal behavior. This paper proposes a combination of the Pearson’s Type IV distribution and the GARCH (1, 1) approach to furnish a new method with superior predictive abilities. The approach is back tested for the entire sample as well as for a holdout sample using rolling windows.