Synthesis of TiO2 based on hydrothermal methods using elevated pressures and microwave conditions

Titanium dioxide (TiO₂), especially in its anatase form, is an effective photocatalyst under ultraviolet (UV) light. The particle size of TiO₂ is a critical factor to determine its photoactivity based on its quantum effectiveness under light irradiations. Thus, nanocrystalline TiO₂ has been widely accepted to significantly enhance this effect. The sol–gel method is generally used to synthesize the anatase form of nanocrystalline TiO₂. In this study, we expanded the synthesis method of TiO₂ to high pressures under direct heating (hydrothermal method) and indirect heating (microwave-assisted method). It was found that pH value is one of the major factors to control nano-sizes of TiO₂ particles, and the neutral condition in all methods is preferable for controlling the sizes of the prepared TiO₂ particles. The microwave-assisted method further improves quality of synthesized nano-size TiO₂ below 10 nm. These results have been confirmed by both the direct size measurement using TEM images and indirect determination using XRD peaks. The collected samples are further analyzed using UV–Vis spectroscopy to identify the particle size-dependent photoreactivity and to confirm the effectiveness of microwave-assisting under neutral conditions. DSC is also a powerful tool to identify the crystalline transition of TiO₂.     

Determination of nifedipine in dog plasma by high‐performance liquid chromatography with tandem mass spectrometric detection

Nifedipine is a dihydropyridine calcium channel blocker used widely in the management of hypertension and other cardiovascular disorders. In this work, a simple, rapid and sensitive liquid chromatography/tandem mass spectrometry method was developed and validated to determine nifedipine in dog plasma using nimodipine as the internal standard. Chromatographic separation was carried out on a C₈ column. The mobile phase consisted of a mixture of acetonitrile, water and formic acid (60:40:0.2, v/v/v) at a flow rate of 0.5 mL/min. Detection was performed on a triple quadrupole tandem mass spectrometer in selected reaction monitoring mode via an atmospheric pressure chemical ionization source. The method has a lower limit of quantification of 0.20 ng/mL with consumption of plasma as low as 0.05 mL. The linear calibration curves were obtained in the concentration range of 0.20–50.0 ng/mL (r = 0.9948). The recoveries of the liquid extraction method were 74.5–84.1%. Intra‐day and inter‐day precisions were 4.1–8.8 and 6.7–7.4%, respectively. The quantification was not interfered with by other plasma components and the method was applied to determine nifedipine in plasma after a single oral administration of two controlled‐release nifedipine tablets to beagle dogs. Copyright © 2013 John Wiley & Sons, Ltd.     

Nucleophilic imidoesterification of dicarbonyl compounds with cyanatobenzenes through C-C bond formation

Under neat conditions,an efficient method for synthesis of imidoesters has been developed using cyanatobenzenes and dicarbonyl compounds.Nucleophilic addition spontaneously occurred between the two kinds of materials at room temperature with yields of up to 90%.A mechanism directed towards to the imidoester formation has been proposed.     

Optimizing Multi-stage Production for an Assembly-Type Supply Chain with Unequal Sized Batch Shipments

This paper studies the multi-stage logistics and inventory problem in an?assembly-type supply chain where a uniform lot size is produced uninterruptedly with a single setup at each stage. Partial lots, or sub-batches, can be transported to next stage upon completion. Unequal sub-batch sizes at each stage follow geometric series and the numbers of sub-batches across stages are allowed to be different. Since the mainline and each branch line of an assembly-type supply chain are series-type supply chains, a model of the series-type supply chain is first established and a model of the assembly-type supply chain is subsequently developed. Optimization algorithms that determine the economic lot sizes, the optimal sub-batch sizes and the number of sub-batches for each stage are developed. The polynomial-time algorithms incorporate the optimality properties derived in the paper to find the lower and upper bounds of the solutions by constructing the solution ranges and then the optimal solutions accordingly.     

Polymeric ytterbium(ii) complex with pyridyl amido ligands

The reaction of potassium pyridyl amido ligand {L = [N(R)(2-C5H3N-6-Me)]–, R = CH2But} with YbI2(thf)2 afforded the linear polymeric complex [K0.5(L)3YbiiK0.5]n, which was characterized by X-ray structure analysis.     

Facile filling of metal particles in small carbon nanotubes for catalysis

A versatile wet chemistry method is developed for filling of subnanometer sized metal particles in carbon nanotubes with a diameter smaller than 1.5 nm. As an example, we showed that a confined bi-component Pd-V catalyst exhibit a higher benzene hydroxylation activity compared with that within multi-walled carbon nanotubes.     

Cs4B4O3F10: First Fluorooxoborate with [BF4] Involving Heteroanionic Units and Extremely Low Melting Point

Herein, a new congruently melting mixed-anion compound Cs₄B₄O₃F₁₀ has been characterized as the first fluorooxoborate with [BF₄] involving heteroanionic units. Compound Cs₄B₄O₃F₁₀ possesses two highly fluorinated anionic clusters and therefore its formula can be expressed as Cs₃(B₃O₃F₆) ⋅ Cs(BF₄). The influence of [BF₄] units on micro-symmetry and structural evolution was discussed based on the parent compound. More importantly, Cs₄B₄O₃F₁₀ shows the lowest melting point among all the available borates and thus sets a new record for such system. This work is of great significance to enrich and tailor the structure of borates using perfluorinated [BF₄] units.     

A Practical Total Synthesis of Taxamairin B

Taxamairin B. a novel rearranged 9(10 ± 20)-abeo-8. 11. 13-triene diterpenoid. has been convergently synthesized by a facile route, which employed the acid catalyzed rearrangement and oxidation of vinyl carbinol as the key steps.