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Daniel E. Lynch Gillian E. Spicer Ian Mcclenaghan 《Journal of heterocyclic chemistry》2005,42(7):1363-1368
Three α‐phenylmalonamides have been prepared by the selective nucleophilic cleavage of 5,7‐dimethyl‐2‐phenyl‐1‐oxo‐1H‐pyrazolo[1,2‐a]pyrazol‐4‐ylium‐3‐olate in solventless microwave syntheses. The three weak nucleophiles employed were aniline, p‐chloroaniline and m‐toluidine. The α‐phenylmalonamides of these three aniline derivatives could not be prepared using the previously reported solvent syntheses via 3‐oxopyrazolo[1,2‐a]pyrazol‐8‐ylium‐1‐olates. All products were characterised using, infrared spectroscopy, 1H nmr and electrospray mass spectrometry. The single crystal X‐ray structures of the starting pyrazolo‐[1,2‐a]pyrazole and α‐phenylmalon‐m‐toluidide are also reported. 相似文献
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Aihara H Alston-Garnjost M Avery RE Barbaro-Galtieri A Barker AR Barnes AV Barnett BA Bauer DA Bengtsson H Bintinger DL Bobbink GJ Bolognese TS Bross AD Buchanan CD Buijs A Cain MP Caldwell DO Clark AR Cowan GD Crane DA Dahl OI Derby KA Eastman JJ Eberhard PH Eisner AM Enomoto R Erné FC Fujii T Gary JW Gorn W Hauptman JM Hofmann W Huth JE Hylen J Kamae T Kaye HS Kees KH Kenney RW Kerth LT Ko W Koda RI Kofler RR Kwong KK Lander RL Langeveld WG Layter JG Linde FL Lindsey CS Loken SC Lu A Lu X 《Physical review letters》1986,57(8):945-948
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Sessler JL Roznyatovskiy V Pantos GD Borisova NE Reshetova MD Lynch VM Khrustalev VN Ustynyuk YA 《Organic letters》2005,7(23):5277-5280
[reaction: see text] Two easy-to-synthesize polypyrrolic 2,5-diamidothiophene Schiff base macrocycles are reported, along with their anion binding properties as determined via UV-vis spectroscopic titrations carried out in dichloroethane. There is a striking difference between the interactions with anions of the two macrocycles, a finding ascribed to differences in their rigidity. For example, the more flexible dipyrromethane-derived macrocycle displays a 1.2:1 hydrogen sulfate versus nitrate selectivity, while its more rigid bipyrrole-derived congener shows a 7.4:1 selectivity in favor to hydrogen sulfate. 相似文献
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Summary Interpretive methods are accepted to give the best possible results for selectivity optimization in HPLC. However the methods are very complex, and most work so far has been detailed academic studies. This paper describes an evaluation of a complete integrated system incorporating peak labelling, modelling of retention behaviour and calculation of response surfaces, with particular emphasis on the retention modelling. The peak labelling section has been discussed previously.A piece-wise quadratic function is investigated for the modelling of retention times across an isoeluotropic plane to effect selectivity optimization in HPLC. This requires 10 data-points on the isoeluotropic plane. The predicted global optimum and local optima are evaluated by comparison of calculated and experimental retention data, for a nine component sample. Seven interstitial points, distributed across the whole plane between the data-points, are similarly evaluated for a related sample. The typical error (in retention time) is less than 2%, often 1%, and the maximum error is 4.2%. At the global optimum the error was found be less than 1.3% for all 9 peaks. 相似文献
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Determination of the total nitrogen content of hard, semihard, and processed cheese by the Kjeldahl method: collaborative study 总被引:1,自引:0,他引:1
The objective of this collaborative study was to determine interlaboratory performance statistics for a modified and optimized version of AOAC Method 920.123 for the determination of the total nitrogen content of hard, semihard, and processed cheese by Kjeldahl analysis. Details included addressing the issues of material homogeneity, test portion size (1 g), quantitative transfer (weighing on to filter paper), ensuring system suitability (nitrogen recoveries), and using AOAC Method 991.20 as the basis for nitrogen analysis. Fifteen laboratories tested 18 pairs of blind duplicate cheese materials with a crude protein content between 18 and 36%. Materials represented hard, semihard, and processed commercial cheeses with a wide range of composition. Statistical performance parameters expressed as crude protein (nitrogen x 6.38), g/100 g, with invalid and outlier data removed were mean = 26.461, repeatability standard deviation (Sr) 0.111, reproducibility standard deviation (S(R)) = 0.153, repeatability relative standard deviation (RSDr) = 0.42%, reproducibility relative standard deviation (RSDR) = 0.58%, repeatability (r) = 0.312, and reproducibility (R) = 0.428. The interlaboratory study results were acceptable and comparable to those for the milk Kjeldahl nitrogen method on a relative nitrogen basis. The Study Directors recommend that this modified method for the determination of total nitrogen in hard, semihard, and processed cheese by Kjeldahl analysis be adopted First Action as an improved method to replace Method 920.123. 相似文献