Zirconium Borohydride - a Versatile Reducing Agent for the Reduction of Electrophilic and Nucleophilic Substrates

Zirconium borohydride, a potential reducing agent, reduces acids, esters, imines to the corresponding alcohols and secondary amines in good yield at room temperature within two hours. This facile reducing property was taken advantage off in the synthesis of pheromones and some novel chiral precursors for asymmetric synthesis.     

Silica Gel Supported Chromium Trioxide: An Efficient Reagent for Oxidative Cleavage of Oximes to Carbonyl Compounds under Mild Condition

A facile, efficient oxidative deblocking of aldoximes and ketoximes to their corresponding aldehydes and ketones have been achieved by using silica gel supported chromium trioxide.     

SYNTHESIS AND SPECTRAL STUDIES OF SOME NEW [(ALKOXYCARBONYLVINYL)ARYL- AND BENZYLSULFONYLMETHYL] SULFONES

Abstract

Some new 1,1,2-trisubstituted ethylenic sulfones have been prepared by the condensation of aryl- and benzylsulfonylmethylsulfonylacetic acid esters with araldehydes.     

AgOTf‐catalyzed transesterification of β‐keto esters

AgOTf proved to be an effective catalyst for the transesterification of β‐keto esters with primary, secondary and tertiary alcohols. The products were obtained in high yield within a reasonable reaction time period. The kinetics of the transesterification reaction were also studied and the reaction was found to follow second‐order kinetics. Copyright © 2012 John Wiley & Sons, Ltd.     

Differential isotope dansylation labeling combined with liquid chromatography mass spectrometry for quantification of intact and N-terminal truncated proteins

The N-terminal amino acids of proteins are important structure units for maintaining the biological function, localization, and interaction networks of proteins. Under different biological conditions, one or several N-terminal amino acids could be cleaved from an intact protein due to processes, such as proteolysis, resulting in the change of protein properties. Thus, the ability to quantify the N-terminal truncated forms of proteins is of great importance, particularly in the area of development and production of protein-based drugs where the relative quantity of the intact protein and its truncated form needs to be monitored. In this work, we describe a rapid method for absolute quantification of protein mixtures containing intact and N-terminal truncated proteins. This method is based on dansylation labeling of the N-terminal amino acids of proteins, followed by microwave-assisted acid hydrolysis of the proteins into amino acids. It is shown that dansyl labeled amino acids are stable in acidic conditions and can be quantified by liquid chromatography mass spectrometry (LC–MS) with the use of isotope analog standards.     

The Interaction of Benzyl Alcohol with Trimethoxyboroxine : Amine Adducts of Triarylboroxines as Model Compounds

The interaction of benzyl alcohol with trimethoxyboroxine has been investigated by hydrogen-1 and carbon-13 NMR and IR spectroscopy. These techniques indicate formation of a weak Lewis acid/base adduct, additionally stabilized by a hydrogen-bonding interaction, which undergoes rapid ligand exchange at room temperature. The system has been modelled by the synthesis and characterization of a series of amine-triarylboroxine adducts. These adducts rapidly undergo ligand dissociation-recombination in solution with ΔG⁺ of ca. 40-50 kJ/mol.     

From Molecular Conformation to Phospholipid Bilayer Organization

Abstract

The structure and the dynamics of D-erythrostearoyl sphingomyelin has been studied by the variable temperature wide-line ³¹P and high-resolution ¹C CP MAS NMR apectroscopy. The results indicate the formation of the highly ordered, relaxed gelphase, and are interpreted based on the conformation of D-erytgrosphingomylin in the unaggregated state.     

Characterisation of PDO olive oil Chianti Classico by non-selective (UV–visible,NIR and MIR spectroscopy) and selective (fatty acid composition) analytical techniques

An authentication study of the Italian PDO (protected designation of origin) extra virgin olive oil Chianti Classico was performed; UV–visible (UV–vis), Near-Infrared (NIR) and Mid-Infrared (MIR) spectroscopies were applied to a set of samples representative of the whole Chianti Classico production area.     

A Direct Spectrofloorimetric Method for the Determination of B-Naphthoxyacetic Acid Residues in Strawberries

Abstract

β-naphthoxyacetic acid (NOA) residues in strawberries have been determined in acetone extracts using direct, first and second derivatives with spectrofluorimetric detection, without clean-up procedures needed. Solvent effects on the spectral characteristics of NOA solutions and their influences on the sensitivity of its variables and instrumental parameters are also studied. A detection limit of 1.14 ng/ml was achieved using the first derivative approach. Strawberries were fortified at different NOA concentrations (10 to 90 ng/ml). Recoveries averaged 87.2% (range 80.16–98.53) at the lower fortification level and 98.36% (range 97.54–99.63) for the higher fortification level.     

Application of the Salicylate Ion Electrode for the Monitoring of the Electroreduction of Salicylic Acid

Abstract

An ion selective electrode is described for measuring the unreacted salicylate ion concentration during the electroreduction of salicylic acid. Conditions for making measurements are discussed.