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61.
Katrin?Anhalt Ines?Sprung Klaus?SchulzeEmail author 《Monatshefte für Chemie / Chemical Monthly》2003,134(12):1593-1606
Summary. Optically active dimethylcyclohexenones, potential building blocks for enantioselective syntheses of various naturally active substances, were prepared. These compounds were obtained by oxidation with KMnO4/Pb(OAc)4 or ozonolysis of the corresponding cyclopentenic precursors, followed by aldol condensation. During the course of the preparation intermediate diols and chiral polyfunctional carbonyl derivatives were separated and identified analytically. 相似文献
62.
Giovanna Bruni Ines Ghione Vittorio Berbenni Andrea Cardini Doretta Capsoni Alessandro Girella Chiara Milanese Amedeo Marini 《Molecules (Basel, Switzerland)》2021,26(11)
The present work is a concrete example of how physico-chemical studies, if performed in depth, are crucial to understand the behavior of pharmaceutical solids and constitute a solid basis for the control of the reproducibility of the industrial batches. In particular, a deep study of the thermal behavior of glipizide, a hypoglycemic drug, was carried out with the aim of clarifying whether the recognition of its polymorphic forms can really be done on the basis of the endothermic peak that the literature studies attribute to the melting of the compound. A number of analytical techniques were used: thermal techniques (DSC, TGA), X-ray powder diffraction (XRPD), FT-IR spectroscopy and scanning electron microscopy (SEM). Great attention was paid to the experimental design and to the interpretation of the combined results obtained by all these techniques. We proved that the attribution of the endothermic peak shown by glipizide to its melting was actually wrong. The DSC peak is no doubt triggered by a decomposition process that involves gas evolution (cyclohexanamine and carbon dioxide) and formation of 5-methyl-N-[2-(4-sulphamoylphenyl) ethyl] pyrazine-2-carboxamide, which remains as decomposition residue. Thermal treatments properly designed and the combined use of DSC with FT-IR and XRPD led to identifying a new polymorphic form of 5-methyl-N-[2-(4-sulphamoylphenyl) ethyl] pyrazine-2-carboxamide, which is obtained by crystallization from the melt. Hence, our results put into evidence that the check of the polymorphic form of glipizide cannot be based on the temperature values of the DSC peak, since such a peak is due to a decomposition process whose Tonset value is strongly affected by the particle size. Kinetic studies of the decomposition process show the high stability of solid glipizide at room temperature. 相似文献
63.
Majerić Elenkov M Primožič I Hrenar T Smolko A Dokli I Salopek-Sondi B Tang L 《Organic & biomolecular chemistry》2012,10(26):5063-5072
A novel activity of halohydrin dehalogenases towards spiroepoxides has been found. The enzyme from Arthrobacter sp. (HheA) catalysed highly regioselective azidolysis of spiroepoxides containing 5, 6 and 7-membered cycloalkane rings, while the enzyme from Agrobacterium radiobacter (HheC), besides high regioselectivity, also displayed moderate to high enantioselectivity (E up to >200) that can be applied for the kinetic resolution of chiral spiroepoxides. The orientations of spiroepoxides in the active site of halohydrin dehalogenases were studied by quantum-chemical calculations and docking simulations. Analyses of the complexes obtained revealed the origins of diastereoselectivity and enantioselectivity of the investigated biotransformations. 相似文献
64.
Hacer Guzlek Ines I.R. Baptista Philip L. Wood Andrew Livingston 《Journal of chromatography. A》2010,1217(40):6230-6240
Literature lists a number of counter-current chromatography (CCC) models that can predict the retention time and to a certain extent the peak width of a solute eluting from a CCC column. The approach described in this paper distinguishes itself from previous reports by relating all model parameters directly to column dimensions and experimental settings. Most importantly, this model can predict a chromatogram from scratch without resorting to traditional calibration using empirical values. The model validation with experimental results obtained across a range of CCC instruments demonstrated that the solute retention time, peak width, and peak resolution could be predicted within reasonable accuracy. Additionally, the effect of several process parameters, such as mobile phase flow rate, rotational speed of the column or β-value, showed that the model is robust and applicable to a wide range of CCC instruments. Overall, this model proved to be a useful tool for parameter estimation and, most significantly, separation optimisation. 相似文献
65.
Xinjie GaiRonald Grigg Ines KöppenJohn Marchbank Visuvanathar Sridharan 《Tetrahedron letters》2003,44(40):7445-7448
A novel palladium catalysed three-component cascade process is described involving allenylation of an aryl iodide to generate a (π-allyl)palladium species which is intercepted by a carbon or nitrogen nucleophile followed by intramolecular Michael addition to afford carbo- and heterocycles in good yield. 相似文献
66.
Rafael Espin Eduardo Fernandez Gustavo Mazcorro Maria Ines Lecich 《European Journal of Operational Research》2007
The object of this paper is to provide a systematic treatment of bargaining procedures as a basis for negotiation. An innovative fuzzy logic approach to analyze n-person cooperative games is developed. A couple of indices, the Good Deal Index and the Counterpart Convenience Index are proposed to characterize the heuristic of bargaining and to provide a solution concept. The indices are examined theoretically and experimentally by analyzing three case studies. The results verify the validity of the approach. 相似文献
67.
Volumetric and transport properties of aerosol-OT reversed micelles containing light and heavy water
Alessandro D'Aprano Ines D. Donato Mario Goffredi Vincenzo Turco Liveri 《Journal of solution chemistry》1992,21(4):323-332
Densities and viscosities of sodium bis(2-ethylhexyl) sulfosuccinate (AOT in-heptane system containing light and heavy water,
as a function of the molar ratio R (R=[H2O or D2O]/[AOT]) were measured at 0, 5, 25 and 40°C. At low R values, the apparent molar volume of deuterium oxide is smaller than
that of light water. The difference is related to the strength of the hydrogen bonding H2O and D2O. The viscosities of both H2O-AOT-n-heptane and D2O-AOT-n-heptane systems were explained in terms of intermicellar interactions mainly governed by hydration of the head groups
of AOT. 相似文献
68.
Controlled Formation of Polymer Nanocapsules with High Diffusion‐Barrier Properties and Prediction of Encapsulation Efficiency 下载免费PDF全文
Ines Hofmeister Prof. Dr. Katharina Landfester Dr. Andreas Taden 《Angewandte Chemie (International ed. in English)》2015,54(1):327-330
Polymer nanocapsules with high diffusion‐barrier performance were designed following simple thermodynamic considerations. Hindered diffusion of the enclosed material leads to high encapsulation efficiencies (EEs), which was demonstrated based on the encapsulation of highly volatile compounds of different chemical natures. Low interactions between core and shell materials are key factors to achieve phase separation and a high diffusion barrier of the resulting polymeric shell. These interactions can be characterized and quantified using the Hansen solubility parameters. A systematic study of our copolymer system revealed a linear relationship between the Hansen parameter for hydrogen bonding (δh) and encapsulation efficiencies which enables the prediction of encapsulated amounts for any material. Furthermore EEs of poorly encapsulated materials can be increased by mixing them with a mediator compound to give lower overall δh values. 相似文献
69.
70.
Ines BaerJohannes van de Kreeke Thomas Peter Josef LinsingerPiotr Robouch Fernando Cordeiro RaposoBeatriz de la Calle 《Trends in analytical chemistry : TRAC》2011,30(7):1177
The International Measurement Evaluation Program (IMEP) organised the IMEP-24 interlaboratory comparison after reports in the media about high levels of lead in toys. The aim of this comparison was to verify the laboratories’ capacity to evaluate trace-element levels in a possible toy-like material according to the European Standard EN 71-3:1994. As test material, it used a former certified reference material containing levels of antimony, arsenic, barium, cadmium, chromium, mercury, lead and selenium around the limits set in the standard.Four expert laboratories confirmed the reference values (Xref) for all elements but Hg, and established a reference value for Hg. The scatter of the results reported by the participants was large, as expected, but showed a close to normal distribution around the reference values for five of the eight trace elements. The spread of results was mainly attributed to sampling and sample preparation.One major issue observed in this exercise was the lack of legislative rules about how to report the result, or, more specifically, the use of the analytical correction, which was introduced in EN 71-3:1994 to achieve consistent interpretation of results and which is to be applied when values are equal to or above the maximum limits set in the standard. Its application by the participants was very inconsistent and led to problems in their evaluation. There is clearly a need for clarification and for more formal regulations with regard to result reporting in order to minimise the risk of confusion.Participants were also asked to give their opinion with regard to the acceptability of the test material for the market. The majority correctly considered the material as non-compliant. However, almost one-third incorrectly assessed the material as compliant. 相似文献