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991.
Three azobenzene pH indicators with amino[bis(ethanesulfonate)] substituents were synthesized and studied by UV–visible absorption spectroscopy in aqueous solution. The indicators exhibit brilliant and distinct colour changes with transitions between pH 1 and 4. Significant changes were observed in the UV–visible spectra on titration with acid with pKa values ranging from 2.2 to 2.8. The indicators demonstrate individual changes in colour as a function of pH. These novel pH indicators complement the existing library of azobenzene indicator dyes and may be useful for environmental situations with high proton concentrations. 相似文献
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995.
In the course of a preliminary study to determine the preparative value and the synthetic applications of the non-heme iron(II) complexes Fe(bpmen)(OTf)2 and Fe(tpa)(OTf)2, in particular the oxidation of alkenes by using hydrogen peroxide as the terminal oxidant, we have found significant differences in catalyst behavior. After several attempts it was clear that the preparative relevance of the oxidation processes was linked to the concentration of the catalyst and optimal results were obtained when the concentration value was 5 mol %. At that concentration, the Fe(bpmen)(OTf)2 catalyst mostly gave rise to mixtures of the epoxide and the trans-dihydroxylation products formed by water-assisted hydrolytic cleavage of the epoxides. Furthermore, the use of the tripodal ligand tpa led to cis dihydroxylation products. When deactivated olefins were used as substrates for the oxidation reaction, the cis-diols were obtained exclusively, although with modest conversions, regardless of the catalyst used. 相似文献
996.
Qun Dang Zhibo Zhang Bingyu Tang Yang Song Ling Wu Tongqian Chen Stephane Bogen Vinay Girijavallabhan David B. Olsen Peter T. Meinke 《Tetrahedron letters》2014
To discover novel nucleosides as potential antiviral agents, 2′-spirolactam and 2′-spiropyrrolidine-containing nucleoside analogs were envisioned. Efficient synthetic routes were developed with an epoxide opening as the key step to establish the quaternary center at the 2′ position, leading to the design and synthesis of uridine analogs 8 and 21, prodrugs 13–16, and cytidine analog 11. 相似文献
997.
Samuel Piña Jr. Diana M. Cedillo Carlos Tamez Nezhueyotl Izquierdo Jason G. Parsons Jose J. Gutierrez 《Tetrahedron letters》2014
Reported here is the reduction of aromatic nitro compounds using sodium borohydride and transition metal sulfides as catalysts. The reaction conditions were optimized using the reduction of nitrobenzene as a model reaction. The catalysts studied were iron sulfide (Fe3S4), copper sulfide (CuS), zinc sulfide (ZnS), cobalt sulfide (Co3S4), and nickel sulfide (NiS). The reduction was monitored using gas chromatography. Quantitative conversions were achieved using Co3S4 and NiS, representing a ten-fold increase in reactivity compared to the non-catalyzed reaction. Fe3S4 and ZnS had no apparent effect on the reduction of nitrobenzene while the reduction using CuS showed a marginal increase. The reduction method was applied to several aryl-nitro derivatives containing either electron-withdrawing or electron-donating groups. Halogen containing aryl-nitro compounds were reduced without dehalogenation. The reduction had no effect on other functional groups such as carboxylic acids, esters, amides, or alkenes, indicating that the reduction is highly chemoselective. 相似文献
998.
Qun Dang Zhibo Zhang Shuangsheng He Yaohong Liu Tongqian Chen Stephane Bogen Vinay Girijavallabhan David B. Olsen Peter T. Meinke 《Tetrahedron letters》2014
To discover novel nucleosides as potential antiviral agents, 4′-spirocyclic phosphono-nucleosides were designed to mimic the monophosphate of R-1479, a known nucleoside inhibitor of HCV NS5B. Bypassing the first kinase step to nucleoside monophosphate is viewed as advantageous since this phosphorylation is often observed as the rate-limiting transformation to the active NTP for many nucleosides. Efficient synthetic routes were developed with a triphenylphosphine–iodine cyclization reaction as the key step to form the tetrahydrofuran 4′-spirocycle. The desired 4′-spirocyclic phosphono-cytidine analogs 12a, 12b, and 16 were prepared in 11 steps. 相似文献
999.
Kevin B. Lavelle Samuel Glover William B. Connick Henry Spitz 《Journal of Radioanalytical and Nuclear Chemistry》2014,301(3):677-683
This paper summarizes a new method for preconcentration of rusty metal samples using DIPEX® Actinide Resin from Eichrom Technologies prior to analysis for trace environmental actinides. This method allows for preconcentration of actinides for which the existing lanthanum coprecipitation method is ill-suited. The new and existing methods were shown to provide comparable results for plutonium analysis. Performance was compared for both lab-prepared controls and environmental samples. Using actinide resin, a mean 238Pu activity of 46 ± 13 % mBq (2σ) was measured, while 238Pu activity of 40 ± 6 % mBq (2σ) was measured using lanthanum coprecipitation. Small quantities of 239+240Pu, likely attributable to fallout, were also detected. 相似文献
1000.
Yoann Fillâtre David Rondeau Antoine Daguin Alain Jadas-Hecart Pierre-Yves Communal 《Analytical and bioanalytical chemistry》2014,406(5):1541-1550
The determination of 256 multiclass pesticides in lavandin essential oil has been performed by liquid chromatography–electrospray ionization tandem mass spectrometry using the scheduled selected reaction monitoring mode available on a quadrupole-linear ion trap mass spectrometer. With the aim of improving the limits of quantification (LOQs) of the target molecules, a sampling step based on evaporation of the essential oil under a nitrogen flow assisted by controlled heating was tested. The LOQs determined in this case were compared with the values obtained with the classic dilution preparation method. With sampling by dilution, 247 pesticides were detected and quantified at low concentration, with 74 % of the pesticides having LOQs of 10 μg L-1 or less. With the evaporation method, a global improvement of the LOQs was observed, with lower LOQs for 92 active substances and LOQs of 10 μg L-1 or less for 82.8 % of the pesticides. Almost twice as many active substances had an LOQ of 1 μg L-1 or less when the evaporation method was used. Some pesticides exhibited poor recovery or high variance caused by volatilization or degradation during the evaporation step. This behavior was evidenced by the case of thiophanate-methyl, which is degraded to carbendazim. Figure
Sampling method by dilution or evaporation in the multiresidue determination of pesticides in essential oils by LC/MS 相似文献