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排序方式: 共有319条查询结果,搜索用时 15 毫秒
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Stefano Vecchio Alessia Catalani Vanessa Rossi Mauro Tomassetti 《Thermochimica Acta》2004,420(1-2):99-104
The thermal behaviour of acetanilide (Ac) and two of its analogues, namely the para-ethoxyacetanilide (p-Eto Ac) and the para-bromoacetanilide (p-Br Ac), which are used as analgesics in the pharmaceutical industry was studied with a simultaneous TG/DSC unit. The examined analgesics showed two endothermic DSC peaks due to melting and vaporization. By combining the experimental TG data with the corresponding reference vapour pressure data obtained with the Antoine equation the plot of P versus v was derived. From the slope of this equation the constant k-value was determined for Ac. Then, using the same k-value the vapour pressures of p-Eto Ac and p-Br Ac were determined in the same temperature range. The vaporization enthalpies for all the studied compounds were obtained from different methods and a very good agreement was found. Vaporization follows a zero-order kinetics. The activation energy of vaporization (Evap) was calculated from the dynamic TG experiments, using the Arrhenius equation. 相似文献
3.
Specific programming of automated HPLC systems allows total on-line qualification, validation and stability monitoring using the concept of deferred standards. Setting up such a process for routine analyses in an automated HPLC system requires specific autosampler programming as well as specific monitoring software. With an autosampler, a double injection procedure is programmed, the first introducing the sample, and the second, a few minutes deferred, the deferred control standard. Two additional compounds are therefore added to the sample before and during the chromatographic process: the intemal standard for sample quantification and the deferred standard for system control. Specific methodologies are described of how to obtain classical quantitative analysis information as well as system qualification validation stability information. Experiments were performed to develop specified methodologies to monitor the quality of quantitative analysis during the life of the column by using the deferred standard concept to probe the effects of column ageing on separation characteristics. 相似文献
4.
Zanoni G Porta A Meriggi A Franzini M Vidari G 《The Journal of organic chemistry》2002,67(17):6064-6069
Regioconvergent synthesis of the key lactone 1 from an equimolar mixture of the two olefins 4 and 5 was achieved by unique Pd(II) chemistry. The synthetic versatility of lactone 1 has been demonstrated in the synthesis of iridoids and of the endo-Corey lactone 2, which is a key intermediate for the F(2)-isoprostane synthesis. Upon exposure of the sodium salts of 4 and 5 to a catalytic amount of Pd(OAc)(2) under oxygen, in the presence of AcOH, an isomeric lactone 12 was obtained in addition to the title compound 1. The Pd(II) lactonization was optimized by fine-tuning all the factors participating in the catalytic cycle: solvent, oxidant, co-oxidant, and Pd(II) source. The Hosokawa's heterobimetallic couple emerged as the catalyst of choice. With a Cu(II)-Pd(II) couple, the redox process was transferred to copper, and the formal oxidation state of palladium remained constant during the reaction. By virtue of this new methodology, lactone 1 was obtained in a rewarding 60% yield, along with isomeric lactone 12 in 30% yield. A detailed mechanistic study was carried out in order to elucidate the formation of lactones 1 and 12. Lactone 1 was formed from either olefin 8 or olefin 10; on the other hand, lactone 12 was formed exclusively from olefin 10. An intramolecular 1,2-acyloxypalladiation was invoked for the transformation of 8 into 1, whereas the pi-allyl complexes 13 and 11 were involved in the transformation of olefin 10 into 12 and 1, respectively. 相似文献
5.
Bacchi Alessia Pelizzi Giancarlo Minardi Giovannina Pistuddi Angelo M. Solinas Costantino Chelucci Giorgio 《Transition Metal Chemistry》2002,27(3):274-278
Metal complexes of general formula M(L)X2 and M(L)X3 [L = (4S,5S)-2,2-dimethyl-4,5-bis{6-[(4,5-dihydro-4-(S)-(1-methylethyl)oxazol-2-yl)pyridin-2-yl]}-1,3-dioxolane] were obtained by reacting, respectively, CoII, CuII, NiII, and ZnII nitrate salts and the RhIII chloride salt, with a chiral C2-symmetric bis(oxazolinylpyridinyl)dioxolane (L) ligand, in MeOH/CHCl3 solution. A single crystal X-ray analysis was carried out on [Ni(L)(OH2)2](NO3)2 · 2H2O and the molecular structure of L was also determined. In the free ligand the two symmetric arms are essentially planar and oriented nearly perpendicular to the dioxolane average plane. In the Ni complex one seven-membered and two five-membered chelation rings are formed. The metal atom also lies on the C2 axis, and two symmetry-related water molecules complete the octahedral coordination environment. Both compounds crystallize in chiral space groups; the ligand crystallizes in orthorhombic system, space group C 2 2 21, Z = 4; the nickel complex crystallizes in tetragonal system, space group P 43 21 2, Z = 4. 相似文献
6.
Presti ML Ragusa S Trozzi A Dugo P Visinoni F Fazio A Dugo G Mondello L 《Journal of separation science》2005,28(3):273-280
Traditional hydrodistillation (HD), supercritical fluid extraction (SFE), organic solvent extraction (SE), and water microwave assisted hydrodistillation (MAHD) techniques were compared and evaluated for their effectiveness in the isolation of rosemary essential oil. The microwave assisted hydrodistillation technique was optimized in terms of both delivered power and time duration. The extracts/distillates were analyzed by GC and GC-MS. Microwave distillation, which exploits the physical action of microwaves on plants, showed a series of advantages over the other approaches: low cost, use of water in sample pre-treatment step, greatly reduced isolation time, and attainment of high quality essential oil distillate. Moreover, the absence of environmental impact of this innovative technique was also emphasized. 相似文献
7.
Vesna Radulovi? Alessia Bacchi Giancarlo Pelizzi Du?an Sladi? Ilija Br?eski Katarina Andjelkovi? 《Monatshefte für Chemie / Chemical Monthly》2006,23(3):681-691
Complexes of Pt(II), Pd(II), and Ni(II) with the condensation derivative of 2-(diphenylphosphino)benzaldehyde and semioxamazide
were synthesized, characterized, and their antimicrobial activity was evaluated. The ligand and the complexes were characterized
by spectroscopic methods with the particular accent on NMR spectral analysis. For the palladium(II) complex, the crystal structure
was determined by X-ray analysis. In all the complexes the ligand is coordinated as a tridentate via a P, N, O donor set. The Pd(II) and Pt(II) complexes have a square planar geometry, whereas the geometry of the Ni(II) complex
is tetrahedral. The ligand showed antibacterial and antifungal activity, which was enhanced upon complexation. 相似文献
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Separation of complex sugar mixtures on a hydrolytically stable bidentate urea‐type stationary phase for hydrophilic interaction near ultra high performance liquid chromatography 下载免费PDF全文
Dorina Kotoni Alessia Ciogli Claudio Villani David S. Bell Francesco Gasparrini 《Journal of separation science》2014,37(5):527-535
A stationary phase bearing both bridged bis‐ureido and free amino groups (USP‐HILIC‐NH2–2.5SP) for high‐speed hydrophilic interaction liquid chromatography separations was prepared using a one‐pot two‐step procedure starting from 2.5 μm totally porous silica particles. Highly polar compounds, such as polyols, hydroxybenzoic acids, and sugars, were successfully analyzed in shorter times and with higher peak efficiency, when compared to results obtained with a bidentate urea‐type column packed with 5 μm particles. Increased sugarophilicity and better peak shape were attested for the USP‐HILIC‐NH2–2.5SP column (100 × 3.2 mm id) when compared with two commercially available UHPLC columns, namely an acquity BEH amide packed with totally porous 1.7 μm microparticles and a HILIC Kinetex column packed with core–shell 2.6 μm particles. Finally, the new column was employed in the separation of complex mixture of sugars (mono‐, di‐, and oligosaccharides) and in the analysis of beer samples. The resulting chromatograms showed good selectivity and overall resolution, while the catalyzing effect of the free amino moieties resulted in excellent peak shapes and in the absence of split peaks due to sugar anomerization phenomena. 相似文献