Tetrahydropyranylation of Alcohols Under Solvent-Free Conditions

A green, efficient, and large-scale method for tetrahydropyranylation of alcohols in the presence of a catalytic amount of pyridinium chloride at room temperature under solvent-free conditions is reported.     

Efficient Method for Iodination of Alcohols using KI/Silica Sulfuric Acid (SSA)

A straightforward and effective procedure for the conversion of benzylic and allylic alcohols to the corresponding iodides using KI/SSA in acetonitrile at room temperature.     

Suitability of Different 13C Solid-state NMR Techniques in the Characterization of Humic Acids

Qualitative and quantitative analyses of humic acids (HAs) with five different ¹³C solid-state NMR techniques were assessed using HAs of various origins and locations. The NMR techniques compared are: (1) direct polarization/magic angle spinning (DP/MAS) at 13 kHz, (2) conventional cross polarization (CP)/MAS at 5 kHz, (3) ramp-CP/MAS at 8 kHz, (4) CP/total sideband suppression (TOSS) at 4.5 kHz, and (5) DP/MAS corrected by CP/spin-lattice relaxation with TOSS. The spectra from the five techniques were first compared qualitatively. Then, each spectrum was divided into eight regions for quantitative evaluation. DP/MAS spectra were used as quantitative references. Ramp-CP/MAS and CP/TOSS spectra gave consistently better results than those of the conventional CP/MAS spectra at a ¹³C frequency of 75 MHz, which were incorrect due to spinning sidebands. CP/MAS at low magnetic fields (22.6 and 50.6 MHz ¹³C frequency) indicated improved integration results but lower resolution. Correction factors calculated by comparison with DP/MAS will be useful to convert the non-quantitative peak areas in the CP/TOSS and ramp-CP/MAS spectra into more quantitative results.     

A Proline-Based Aminophosphinic Acid Ligand and It’s Vanadyl Complex: Synthesis,Characterization and In Vitro Inhibitory Effects on α-Amylase And α-Glucosidase

Abstract

A proline-based aminophosphinic acid ligand and it's vanadium complex have been synthesized and characterized by spectroscopic techniques. The inhibitory activity on pancreatic α-amylase and Baker's yeast α-glucosidase has been examined in vitro. The novel complex showed more inhibitory potency against pancreatic α-amylase and Baker's yeast α-glucosidase compared to acarbose as an antidiabetic drug.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Thermal and structural studies of zinc zirconate nanoscale composite derived from sol–gel process

In the present investigation, a novel synthetic zinc zirconate nanocomposites were prepared by a sol–gel technique using a very stable sol containing zirconium acetylacetonate, zinc acetate, monoethanolamine, and 1,3-propanediol as chelating agent. Thermal analysis results indicated that the decomposition of zinc zirconate precursors occurred at 225 and 234 °C. The influence of thermal annealing (temperatures and duration) on their structural properties has been studied by means of X-ray diffraction and Fourier transform-infrared spectroscopy techniques. The results indicated that a higher percent of zinc zirconate is formed at 800 °C and reached maximum at 1,000 °C in 120 min. The morphology, composition, and bandgap properties of zinc zirconate nanoparticles were characterized by transmission electron microscope, scanning electron microscope (SEM), Energy-dispersive X-ray spectroscopy, and ultraviolet diffiuse reflectance. The SEM observation showed that average grain size of zinc zirconate nanopowders was 58 nm. The optical results revealed maximum absorbances at 394, 413, and 438 nm for ZnZrO₃ sample annealed at 400, 800, and 900 °C for 30 min, respectively. This is an indication that the nanopowder can absorb lights in the higher wavelength.     

Zirconium Phosphate Nanoparticles for Solvent Free Acetylation of Phenols and Salicylic Acid: An Efficient and Eco‐friendly Solid Acid Catalyst for Synthesis of Acetyl Salicylic Acid (Aspirin)

A facile synthesis of zirconium phosphate (ZP) nanoparticles as an effective, eco‐friendly and recyclable solid acid catalyst were studied. PVA was used as the organic matrix which is the dispersing agent and acted as a template for the nanoparticle. It seems H‐bonds between ZP and PVA along polymer chains play an important role in the better dispersion of in situ formed ZP. The catalyst was characterized by several instrumental techniques such as BET, ICP‐OES, XRD, FT‐IR, SEM and TEM. The TPD‐NH₃ analysis suggests the presence of reasonable amount of Brönsted acid sites. The acidic properties of catalyst were studied in acetylation of phenols by acetic anhydride (AA), specifically synthesis of acetylsalicylic acid (ASA), commonly known as Aspirin, from salicylic acid (SA). The effects of reaction time, reaction temperature, mole ratio of reactants, as well as amount of catalysts on the synthesis of ASA were investigated, and the reaction conditions were therefore optimized. The excellent yield (96%) of the ASA was obtained under optimized reaction conditions. The catalyst was recovered from reaction media and reused for 4 times after that with a consistent high yield.     

Second law analysis for nanofluid flow in mini-channel heat sink with finned surface: a study on fin geometries

Journal of Thermal Analysis and Calorimetry - In this numerical work, a second law analysis is carried out for the nanofluid flow and heat transfer in the mini-channel with finned surface. The...     

Electrochemically Induced Diels‐Alder Reaction: An Overview

One of the most important name reactions in organic chemistry, is the Diels‐Alder cycloaddition reaction. It is a chemical reaction between a conjugated diene and a substituted alkene, commonly termed the dienophile to construct a substituted cyclohexene derivative. It is the stereotypical example of a pericyclic reaction with a concerted mechanism. In synthesis, the use of electricity instead of stoichiometric amounts of oxidant or reducing agents is definitely appealing for economic, ecological and selective, reasons. In this review, we try to underscore the combination of the electrosynthesis with Diels‐Alder cycloaddition reaction to establish of a powerful synthetic tool which may encourage synthetic organic chemists to use it in the future.     

Selective extraction of clonazepam from human plasma and urine samples by molecularly imprinted polymeric beads

A molecularly imprinted polymer (MIP) based on free‐radical polymerization was prepared with 1‐(N,N‐biscarboxymethyl)amino‐3‐allylglycerol and N,N‐dimethylacrylamide as functional monomers, N,N‐methylene diacrylamide as the cross‐linker, copper ion‐clonazepam as the template and 2,2‐azobis(2‐methylbutyronitrile) as the initiator. The imprinted polymer was characterized by Fourier transform infrared spectroscopy, elemental analysis, thermogravimetric analysis, and SEM. The MIP of agglomerated microparticles with multipores was used for SPE. The imprinted polymer sorbent was selective for clonazepam. The optimum pH and sorption capacity were 5 and 0.18 mg/g at 20°C, respectively. The profile of the drug uptake by the sorbent reflects good accessibility of the active sites in the imprinted polymer sorbent. The MIP‐SPE was the most feasible technique for the extraction of clonazepam with a high recovery from human plasma and urine samples.     

Isocyanide‐Based Multicomponent Synthesis of Functionalized 2,6‐Dioxohexahydropyrimidines in 1 M Aqueous Glucose

An effective route to novel 2,6‐dioxohexahydropyrimidines is described. This involves reaction of alkyl isocyanides and dialkyl acetylenedicarboxylates in the presence of N,N′‐dimethylurea in 1M aq. glucose.