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351.
Carr JL Sejberg JJ Saab F Holdom MD Davies AM White AJ Leatherbarrow RJ Beavil AJ Sutton BJ Lindell SD Spivey AC 《Organic & biomolecular chemistry》2011,9(19):6814-6824
Aspercyclide A (1) is a biaryl ether containing 11-membered macrocyclic natural product antagonist of the human IgE-FcεRI protein-protein interaction (PPI); a key interaction in the signal transduction pathway for allergic disorders such as asthma. Herein we report a novel approach to the synthesis of the C19 methyl ether of aspercyclide A, employing a Pd(0)-catalysed, fluorous-tagged alkenylgermane/arylbromide macrocyclisation (germyl-Stille reaction) as the key step, and evaluation of both enantiomers of this compound via ELISA following optical resolution by CSP-HPLC. A crystal structure for germyl hydride 27 is also reported. 相似文献
352.
Soni Mehul N. Kumar Sivakumar Prasanth Johar SR Kaid Pandya Himanshu A. 《Structural chemistry》2019,30(4):1323-1334
Structural Chemistry - Rheumatoid arthritis (RA) is an autoimmune disorder that causes chronic inflammation with periodic bursts of activity in multiple synovial joints which lead to irreversible... 相似文献
353.
Belgacem O Buchacher A Pock K Josic D Sutton C Rizzi A Allmaier G 《Journal of mass spectrometry : JMS》2002,37(11):1118-1130
Human plasma-derived antithrombin III (AT-III), factor IX (FIX) and vitronectin (VN) were characterized as native glycoproteins and in their de-N-glycosylated form by means of MALDI mass spectrometry. The average molecular masses of the three complex glycoproteins were determined applying internal calibration with high-mass, well-defined protein calibrants. Internal calibration generated for the 47 kDa yeast protein enolase a mass precision in the continuous and delayed extraction mode of +/-0.12 and +/-0.022%, respectively. The achievable mass accuracy for such a high-mass, unmodified protein was in the range of 0.02% in the continuous mode, which turned out to be better than in the delayed extraction mode. Purification of all (glyco) proteins (even the calibration proteins) by means of ZipTip technology and direct elution with a solvent system containing the appropriate MALDI matrix turned out to be a prerequisite to measure the exact molecular masses with an internal calibration. The average molecular masses of the two different forms of AT-III, namely AT-III(alpha) and AT-III(beta), were shown to be 57.26 and 55.04 kDa, respectively. The 2.22 kDa mass difference is attributed to the known difference in carbohydrate content at one specific site (Asn-135). After exhaustive de-N-glycosylation (by means of PNGase F) of the alpha- and beta-form and subsequent MALDI-MS analysis, average molecular masses of 48.96 and 48.97 kDa, respectively, were obtained. These values are in good agreement (-0.15%) with the calculated molecular mass (49.039 kDa) of the protein part based on SwissProt data. The molecular mass of the heavily post-translational modified glycoprotein FIX was found to be 53.75 kDa with a peak width at 10% peak height of 4.5 kDa, because of the presence of many different posttranslational modifications (N- and O-glycosylation at multiple sites, sulfation, phosphorylation, hydroxylation and numerous gamma-carboxyglutamic acids). MALDI-MS molecular mass determination of the native, size-exclusion chromatography-purified, VN sample revealed that the glycoprotein was present as dimer with molecular mass of 117.74 kDa, which could be corroborated by non-reducing SDS-PAGE. After sample treatment with guanidine hydrochloride and mass spectrometric analysis, a single, new main component was detected. The molecular mass turned out to be 59.45 kDa, representing the monomeric form of VN, known as V75. The determined molecular mass value was shown to be on one hand lower than from SDS-PAGE and on the other higher than the calculated amino acid sequence molecular mass (52 277 Da), pointing to the well-known SDS-PAGE bias and to considerable post-translational modifications. Further treatment of the sample with a reducing agent and subsequent MALDI-MS revealed two new components with molecular masses of 49.85 and 9.41 kDa, corresponding to V65 and V10 subunits of VN. PNGase F digest of the V75 and V65 units and MS analysis, exhibiting a molecular mass reduction of 6.37 kDa in both cases, verified the presence of a considerable amount of N-glycans. 相似文献
354.
Jack B. Levy Steven B. Sutton Ronald E. Olsen 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):601-604
Carbon-oxygen bonds ortho to a phosphoryl group in triarylphosphine oxides undergo cleavage when the oxides are either fused with potassium hydroxide or treated with potassium tert-butoxide in refluxing toluene, presumably through a nucleophilic addition-elimination mechanism. Thus, bis(2-hydroxyphenyl)phenylphosphine oxide is produced along with the expected 2-phenoxyphenyl(phenyl)phosphinic acid from 10-phenyl-10H-phenoxaphosphine 10-oxide. The latter starting material is also produced, together with bis(2-hydroxyphenyl)phenylphosphine oxide, when bis(2-methoxyphenyl)phenylphosphine oxide is fused with potassium hydroxide. Fusion of bis(2-methoxyphenyl)phenylphosphine oxide with sodium hydroxide, however, yields 2-hydroxyphenyl(phenyl)phosphinic acid. Ab initio quantum chemical studies confirm that the downfield 31P chemical shift that is observed in 2-phosphinylphenols is due to hydrogen bonding to the phosphoryl group. 相似文献
355.
Oliver J. Sutton 《Numerical Algorithms》2017,75(4):1141-1159
We present a 50-line MATLAB implementation of the lowest order virtual element method for the two-dimensional Poisson problem on general polygonal meshes. The matrix formulation of the method is discussed, along with the structure of the overall algorithm for computing with a virtual element method. The purpose of this software is primarily educational, to demonstrate how the key components of the method can be translated into code. 相似文献
356.
Rayleigh scattering cross sections are measured for nine combustion species (Ar, N2, O2, CO2, CO, H2, H2O, CH4, and C3H8) at wavelengths of 266, 355, and 532 nm and at temperatures ranging from 295 to 1525 K. Experimental results show that, as laser wavelengths become shorter, polarization effects become important and the depolarization ratio of the combustion species must be accounted for in the calculation of the Rayleigh scattering cross section. Temperature effects on the scattering cross section are also measured. Only a small temperature dependence is measured for cross sections at 355 nm, resulting in a 2-8% increase in cross section at temperatures of 1500 K. This temperature dependence increases slightly for measurements at 266 nm, resulting in a 5-11% increase in cross sections at temperatures of 1450 K. 相似文献
357.