Preparative isolation of (+)-beta-eudesmol fromAmyris balsamifera

Summary Optically pure (+)-beta-eudesmol is a possible starting material for the synthesis of several termite defense compounds. A two step procedure for the isolation of gram quantities of (+)-beta-eudesmol from commercially availableAmyris balsamifera oil (syn. West Indian sandalwood oil), containing 8% beta-eudesmol, was developed. Step one consisted of an efficient vacuum distillation of the total oil. Step two was a medium pressure LC separation with an AgNO₃ impregnated silica gel stationary phase. Several other separation procedures failed due to the presence of many closely related sesquiterpene alcohols (75% of the oil).     

Single-frequency, single-mode, plane-polarized ytterbium-doped fiber master oscillator power amplifier source with 264 W of output power

We present a single-frequency, single-mode, plane-polarized ytterbium-doped all-fiber master oscillator power amplifier source at 1060 nm generating 264 W of continuous-wave output power. The final-stage amplifier operated with a high gain of 19 dB and a high conversion efficiency of 68%. There was no evidence of rollover from stimulated Brillouin scattering even at the highest output power, and the maximum output was limited only by the available pump power.     

Synthesis of Novel Functionalized 4-Aza-2,3-Didehydropodophyllotoxin Derivatives with Potential Antitumor Activity

Novel arylamino alcohols were synthesized and these alcohols were used to prepare 12 novel N-(2-hydroxy-ethyl)-2,3-didehydroazapodophyllotoxins, in one step, by simple reflux in ethanol. Isolated yields in the range of 50-70% were obtained.     

Rhenium complexes of tris(pyrazolyl)methanes and sulfonate derivative

The trioxo [ReO(3){SO(3)C(pz)(3)}] (1) (pz = pyrazolyl) and oxo [ReOCl{SO(3)C(pz)(3)}(PPh(3))]Cl (2) compounds with tris(pyrazolyl)methanesulfonate were obtained by treatment of Re(2)O(7) or [ReOCl(3)(PPh(3))(2)], respectively, with Li[SO(3)C(pz)(3)], whereas [ReCl(3){HC(pz)(3)}] (3), [ReCl(3){HC(3,5-Me(2)pz)(3)}] (4) and [ReCl(4){eta(2)-HC(pz)(3)}] (5) were prepared by reaction of [ReOCl(3)(PPh(3))(2)] (3,4) or [ReCl(4)(NCMe)(2)] (5) with hydrotris(pyrazolyl)methane HC(pz)(3) (3,5) or hydrotris(3,5-dimethyl-1-pyrazolyl)methane HC(3,5-Me(2)pz)(3) (4). [ReO{SO(3)C(pz)(3)}{OC(CH(3))(2)pz}][ReO(4)] 6, with a chelated pyrazolyl-alkoxide, was derived from an unprecedented ketone-pyrazolyl coupling on reaction of crude 1 with acetone. The compounds have been characterized by elemental analyses, IR and NMR spectroscopies, FAB-MS spectrometry and cyclic voltammetry and, in the case of 5 and 6, also by single-crystal X-ray diffraction. The electrochemical E(L) Lever parameter has been estimated, for the first time, for the SO(3)C(pz)(3)(-) and oxo ligands allowing the measurement of their electron-donor character and comparison with other ligands. Compounds 1, 2 and 6 appear to be the first tris(pyrazolyl)methanesulfonate complexes of rhenium to be reported.     

Phenolic molecules in virgin olive oils: a survey of their sensory properties, health effects, antioxidant activity and analytical methods. An overview of the last decade

Among vegetable oils, virgin olive oil (VOO) has nutritional and sensory characteristics that to make it unique and a basic component of the Mediterranean diet. The importance of VOO is mainly attributed both to its high content of oleic acid a balanced contribution quantity of polyunsaturated fatty acids and its richness in phenolic compounds, which act as natural antioxidants and may contribute to the prevention of several human diseases. The polar phenolic compounds of VOO belong to different classes: phenolic acids, phenyl ethyl alcohols, hydroxy-isochromans, flavonoids, lignans and secoiridoids. This latter family of compounds is characteristic of Oleaceae plants and secoiridoids are the main compounds of the phenolic fraction. Many agronomical and technological factors can affect the presence of phenols in VOO. Its shelf life is higher than other vegetable oils, mainly due to the presence of phenolic molecules having a catechol group, such as hydroxytyrosol and its secoiridoid derivatives. Several assays have been used to establish the antioxidant activity of these isolated phenolic compounds. Typical sensory gustative properties of VOO, such as bitterness and pungency, have been attributed to secoiridoid molecules. Considering the importance of the phenolic fraction of VOO, high performance analytical methods have been developed to characterize its complex phenolic pattern. The aim of this review is to realize a survey on phenolic compounds of virgin olive oils bearing in mind their chemical-analytical, healthy and sensory aspects. In particular, starting from the basic studies, the results of researches developed in the last ten years will be focused.     

Electrochemical and electron spin resonance studies of selected benzazolo[3,2-a]quinolinium salts

The electrochemical reduction of the chloride or perchlorate salts of benzazolo[3,2-a]quinolinium ion and several of its analogues is reported. The compounds studied are the perchlorate salt of 3-nitrobenzothiazolo-and 3-nitro-9-methoxybenzothiazolo[3,2-a]quinolinium, and the chloride salts of 7-ethyl-, 3-nitro-7-methyl-, 3-nitro-7-ethyl-, 3-nitro-7-isopropyl-, 3-nitro-7-butyl- and 3-nitro-7-benzylbenzimidazolo[3,2-a]-quinolinium, respectively. Cyclic voltammetry of the corresponding 3-nitrobenzothiazolo[3,2-a]quinolinium derivatives in N,N-dimethylformamide shows an irreversible peak potential at -0.6 and a quasi-reversible peak at -(1.2–1.3) volts, respectively, relative to the standard calomel electrode. In contrast, the corresponding 3-nitrobenzimidazolo[3,2-a]quinolinium derivatives show, in general, reversible peaks at near -0.8 and -(1.2–1.4) volts, respectively. Upon electrolytic reduction, only the nitro-substituted derivatives produced observable electron paramagnetic resonance electron spin resonance spectra. This observation is explained in terms of the stabilization of the radicals produced by the nitro group. Theoretical MM+/AM1/UHF calculations support the idea that the larger nitrogen splitting is caused by N-12 and the minor splittings by N-7 in the benzimidazolo[3,2-a]quinolinium ion series.     

Analysis of metallic nanoparticles embedded in thin film semiconductors for optoelectronic applications

This paper reports about a study of the local plasmonic resonance (LSPR) produced by metal nanoparticles embedded in a dielectric or semiconductor matrix. It is presented an analysis of the LSPR for different nanoparticle metals, shapes, and embedding media composition. Metals of interest for nanoparticle composition are Aluminum and Gold. Shapes of interest are nanospheres and nanotriangles. We study in this work the optical properties of metal nanoparticles diluted in water or embedded in amorphous silicon, ITO and ZnO as a function of size, aspect-ratio and metal type. Following the analysis based on the exact solution of the Mie theory and DDSCAT numerical simulations, it is presented a comparison with experimental measurements realized with arrays of metal nanospheres. Simulations are also compared with the LSPR produced by gold nanotriangles (Au NTs) that were chemically produced and characterized by microscope and optical measurements.     

Molybdenum- and tungsten(II) monometallic 3-(2-pyridyl)pyrazole and bimetallic 3-(2-pyridyl)pyrazolate complexes

Molybdenum and tungsten complexes containing the pypzH (3-(2-pyridyl)pyrazole) ligand as a chelating bidentate are prepared: [Mo(CO)(4)(pypzH)], cis-[MoBr(η(3)-allyl)(CO)(2)(pypzH)], cis-[MoCl(η(3)-methallyl)(CO)(2)(pypzH)], [MI(2)(CO)(3)(pypzH)] (M = Mo, W) from [Mo(CO)(4)(NBD)] or the adequate bis(acetonitrile) complexes. The deprotonation of the molybdenum allyl or methallyl complexes affords the bimetallic complexes [cis-{Mo(η(3)-allyl)(CO)(2)(μ(2)-pypz)}](2) or [cis-{Mo(η(3)-methallyl)(CO)(2)(μ(2)-pypz)}](2) (μ(2)-pypz = μ(2)-3-(2-pyridyl-κ(1)N)pyrazolate-2κ(1)N). The allyl complex was subjected to an electrochemical study, which shows a marked connection between both metallic centres through the bridging pyridylpyrazolates.     

Upcycling Rocha do Oeste Pear Pomace as a Sustainable Food Ingredient: Composition,Rheological Behavior and Microstructure Alone and Combined with Yeast Protein Extract

This work explores the potential of Rocha do Oeste pear pomace to be used as a sustainable and healthy food ingredient. Moreover, the enrichment with yeast protein extract (YPE) may be useful to design innovative food products. The main goals of this study were to assess pear pomace concerning: (i) chemical composition and antioxidant capacity; (ii) rheology, texture, and microstructure characterization (alone or enriched with YPE), before and after heating. The results showed that pear pomace was a rich source of dietary fibers (74.5% DW), with phenolic compounds (3.9 mg chlorogenic acid equivalents/g dry weight), also presenting antiradical activity (3.90 μmol Trolox equivalents/g DW). Pear pomace showed a shear thinning behavior and a typical soft-gel behavior, which was not affected by YPE enrichment, thus suggesting that YPE did not affect pear pomace technological properties. Thermal treatment also did not alter pear pomace rheological properties. YPE addition induced a decrease in the apparent viscosity and a destabilizing effect, compared to the samples that were subjected to thermal processing. These results highlight the importance of pear pomace and the use of YPE for protein enrichment, opening new opportunities for their exploitation.