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101.
Dale Pace William E. Hunter Riz Shakir Lowell D. Kispert Jerry L. Atwood 《Journal of chemical crystallography》1980,10(5-6):115-121
The crystal structure of dichlorofluoroacetamide has been determined from three-dimensional counter data, and refined by full-matrix least-squares techniques. The crystals belong to the monoclinic space groupP21 /c and have the unit-cell parametersa = 10.207(4),b = 5.729(2),c = 9.971(4) Å, = 105.21(8) °, andD
x
= 1.72 g cm-3. The structural refinement gave a finalR factor of 0.067 from 440 observed reflections. The compound has nearly equal disorder of the -Cl2F moiety about the C-C bond axis with occupancy factors of the two fragments being 0.48 and 0.52. 相似文献
102.
A method for determining long-chain branching frequency and molecular weight averages for unfractionated low-density polyethylene (LDPE) by the combined use of gel-permeation chromatography (GPC) and intrinsic viscosity data has been reported (GPC–IV method). The method assumes that the number of long branches λ per unit molecular weight is a constant independent of molecular weight. Recent data reported on λ as a function of molecular weight M in commercial LDPE indicate that this assumption is not generally valid, and concern has been expressed as to the size of the errors in molecular weights calculated using this assumption. The errors associated with assuming that λ is constant were evaluated in this study by first determining the way in which λ varies with M for two typical commerical LDPE resins by fractionation and application of the GPC–IV method to representative fractions. The experimentally determined relations between λ and M were then employed in the calculation of molecular weight and molecular size averages from GPC–IV data on the original unfractonated samples. Although it was found that λ increases with molecular weight for both samples, the results indicate that the error involved in assuming that λ is a constant is no greater than the precision with which molecular weight averages can be evaluated by GPC. 相似文献
103.
104.
105.
James W. Pavlik Heather S T. Martin Karen A. Lambert Jennifer A. Lowell Vikki M. Tsefrikas Cheryl K. Eddins Naod Kebede 《Journal of heterocyclic chemistry》2005,42(2):273-281
5‐Phenylisoxazole ( 4 ) and 4‐phenylisoxazole ( 22 ) underwent phototransposition to 5‐phenyloxazole ( 5 ) and 4‐phenyloxazole ( 24 ) respectively. Labeling with deuterium or methyl confirmed that these phototranspositions occurred via the P4 pathway which involves only interchange of the N2 and C3 ring position. Thus, 4‐deuterio‐5‐phenylisoxazole ( 4‐4d ), 4‐methyl‐5‐phenylisoxazole ( 10 ), and 5‐methyl‐4‐phenylisoxazole ( 23 ) phototransposed to 4‐deuterio‐5‐phenyloxazole ( 5‐4d ), 4‐methyl‐5‐phenyloxazole ( 11 ), and 5‐methyl‐4‐phenyloxazole ( 25 ) respectively. In addition to phototransposition, isoxazoles 4, 10 , and 23 also underwent photo‐ring cleavage to yield benzoylacetonitrile (9), α‐benzoylpropionitrile ( 15 ), and aceto‐α‐phenylacetonitrile ( 26 ) respectively. Irradiation of 5‐phenyl‐3‐(trifluoromethyl)isoxazole ( 16 ) in acetonitrile led to 5‐phenyl‐2‐(trifluoromethyl)oxazole ( 17 ), the P4 phototransposition product. Irradiation of 16 in methanol led to a substantial decrease in the yield of 17 and to the formation of a mixture of (E) and (Z)‐2‐methoxy‐2‐(trifluoromethyl)‐3‐benzoylaziridines 18a and 18b . 相似文献
106.
Lowell M. Schwartz 《Analytica chimica acta》1980,122(3):291-301
When more than one parameter is found by a least-squares calculation, the statistical uncertainties of the parameters are generally interdependent. If the uncertainty of one such parameter is quoted as a confidence interval based on the standard error estimate of that parameter and the Student t-statistic, this interval tends to be an underestimate. A suggestion is made to quote more conservative parameter uncertainties as the extreme points on the 95% joint confidence ellipsoid and it is shown that these joint parametric uncertainties are easily calculated from the standard error estimates. Both linear and nonlinear multiple regression are discussed. Nonlinear parameter uncertainties are found after an iterative search for the minimum sum-of-squares of residuals; searches by the Gauss and simplex methods are considered. A joint parametric uncertainty calculation is illustrated by a four-parameter nonlinear regression involving a pH potentiometric titration. 相似文献
107.
108.
Robert I. Gelb Lowell M. Schwartz 《Journal of inclusion phenomena and macrocyclic chemistry》1989,7(5):537-543
A spectrophotometric method is used to determine formation constants of complexes of-cyclodextrin, the 2,6-di-O-methylated and 2,3,6-tri-O-methylated derivatives of-cyclodextrin as hosts with adamantan-1-ylammonium, adamantan-2-ylammonium and adamantan-1-ylmethylammonium as substrate species. The spectrophotometric method uses methyl orange anion and acid forms as indicator species. Complexes of the cyclodextrins with these species are determined as well as with the adamantane derivatives. Standard enthalpies and entropies of formation of all complexes are calculated from the temperature variation of the equilibrium constants.-Cyclodextrin and its 2,6-O-methyl derivative have comparable complex strengths with adamantaneammonium substrates and these strengths are about two orders of magnitude stronger than the corresponding complexes of the permethylated derivative. Thermodynamic parameters are interpreted in terms of differing intramolecular properties of the cyclodextrin complexes. 相似文献
109.
Robert I. Gelb Lowell M. Schwartz 《Journal of inclusion phenomena and macrocyclic chemistry》1989,7(4):465-476
A pH potentiometric method is used to measure complex formation constants of aqueous alpha- and/or beta-cyclodextrin with several carboxylic acids and carboxylate anions: butyric acid/butyrate; valeric acid/valerate; hexanoic acid/hexanoate; octanoic acid/octanoate; decanoic acid/decanoate; cyclohexanecarboxylic acid/cyclohexanecarboxylate and benzoic acid/benzoate. Standard enthalpies and entropies of complex formation are calculated from the temperature dependencies of the equilibrium constants. These thermodynamic parameters of the alpha-cyclodextrin complexes largely conform to a correlation based on complexes with other substrate species previously reported. Both standard enthalpies and entropies of formation of beta-cyclodextrin complexes are found to be more positive than the corresponding complexes of alpha-cyclodextrin with the same substrates. These observations lead to insights into the bonding mechanism of cyclodextrin complexation. 相似文献
110.
Guo L Kozlosky CJ Ericsson LH Daniel TO Cerretti DP Johnson RS 《Journal of the American Society for Mass Spectrometry》2003,14(9):1022-1031
The epidermal growth factor receptor (EGFR) is a receptor tyrosine kinase involved in the regulation of growth in many animal cells, including cancer cells. Phosphorylation of specific tyrosine residues within the cytoplasmic domain of EGFR is part of the initial activation process that occurs upon ligand binding, and these phosphotyrosine residues subsequently serve as docking sites for intracellular signaling molecules. To study the phosphorylation on each individual site, EGFR generated from a human epidermoid carcinoma cell line (A431) was analyzed by mass spectrometry. Liquid chromatography combined with tandem mass spectrometry (LC/MS/MS) was used to identify the tryptic phosphopeptides and their sites of phosphorylation (Y992, Y1045, Y1068, Y1086, S1142, Y1148, and Y1173). Ion intensities for the phosphorylated and unphosphorylated tryptic peptides containing the sites of phosphorylation were measured, and the intensity ratios were used to assess the degree of phosphorylation at each site. Ligand concentrations were varied for epidermal growth factor (EGF) and transforming growth factor alpha (TGF alpha) as stimuli, and all of the EGFR tyrosine sites were consequently found to exhibit increased levels of phosphorylation, although at different rates and to different extents. Phosphorylation of Y992 appeared to plateau at lower concentrations of ligand, whereas the other sites continued to have increased phosphorylation throughout a wide range of concentrations. Only small differences could be detected between the EGF and the TGF alpha-induced EGFR phosphorylation. Pretreatment of A431 cells with a small molecule EGFR inhibitor nearly eliminated the ligand-induced phosphorylation on all of the sites except for Y992 and Y1068. 相似文献