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1.
B. MacMillan M. Halse M. Schneider L. Fardy Y. H. Chui B. J. Balcom 《Applied magnetic resonance》2002,22(2):247-256
Magnetic resonance imaging has rarely been applied to rigid polymeric materials, due primarily to the strong dipolar coupling and short signal lifetimes inherent in these materials. SPRITE (single point ramped imaging withT 1 enhancement) (B. J. Balcom, R. P. MacGregor, S. D. Beyea, D. P. Green, R. L. Armstrong, T. W. Bremner: J. Magn. Reson. A123, 131–134, 1996) is particularly well suited to imaging solid materials. With SPRITE, the only requirement is thatT 2* be long enough so that the signal can be phase-encoded. The minimum phase encoding time is limited by the maximum gradient strength available and by the instrument deadtime. At present this is usually tens of microseconds and will only improve with refinements in technology. We have used the SPRITE sequence in conjunction with raising the sample temperature to obtain images of rigid polymers that have largely frustrated conventional imaging methods. This approach provides a straightforward and reliable method for imaging a class of samples that, up until now, have been very difficult to image. 相似文献
2.
KL Britton HF Rogers Y Asano T Dairi Y Kato TJ Stillman DW Rice 《Acta crystallographica. Section D, Biological crystallography》1998,53(4):124-126
The novel NAD+-linked opine dehydrogenase from a soil isolate Arthrobacter sp. strain 1C belongs to an enzyme superfamily whose members exhibit quite diverse substrate specificites. Crystals of this opine dehydrogenase, obtained in the presence or absence of co-factor and substrates, have been shown to diffract to beyond 1.8 ? resolution. X-ray precession photographs have established that the crystals belong to space group P21212, with cell parameters a = 104.9, b = 80.0, c = 45.5 ? and a single subunit in the asymmetric unit. The elucidation of the three-dimensional structure of this enzyme will provide a structural framework for this novel class of dehydrogenases to enable a comparison to be made with other enzyme families and also as the basis for mutagenesis experiments directed towards the production of natural and synthetic opine-type compounds containing two chiral centres. 相似文献
3.
The reactions of phenyl-, o-chlorophenyl-, p-chlorophenyl-, 3,4-dichlorophenyl-, p-fluoro- and p-anisylmaleic anhydrides with trimethylsilyl azide are described. In all cases mixtures of isomeric 4- and 5-aryl-2H-1,3-(3H)oxazine-2,6-diones are obtained after hydrolysis with the 4-isomer predominating. The yield of 5-isomer is greatest for o-chlorophenyl maleic anhydride, and substantial for other arylmaleic anhydrides, indicating increased importance of steric effects in these reactions, in contrast to previously reported syntheses of methyl and halo-substituted oxazine-diones, where electronic factors appeared dominant. 相似文献
4.
Ronald L. Cerny Denise K. MacMillan Michael L. Gross Alan K. Mallams Birendra N. Pramanik 《Journal of the American Society for Mass Spectrometry》1994,5(3):151-158
Molecular weights of macrolide antibiotics can be determined from either (M + H)+ or (M + Met)+, the latter desorbed from alkali metal salt-saturated matrices. The ion chemistry of macrolides, as determined by tandem mass spectrometry (MS/MS), is different for ions produced as metallated than those formed as (M + H)+ species. An explanation for these differences is the location of the charge. For protonated species, the charge is most likely situated on a functional group with high proton affinity, such as the dimethylamino group of the ammo sugar. The alkali metal ion, however, is bonded to the highly oxygenated aglycone. As a result, the collision-activated dissociation spectra of protonated macrolides are simple with readily identifiable fragment ions in both the high and low mass regions but no fragments in the middle mass range. In contrast, the cationized species give complex spectra with many abundant ions, most of which are located in the high mass range. The complementary nature of the fragmentation of these two species recommends the study of both by MS/MS when determining the structure or confirming the identity of these biomaterials. 相似文献
5.
Ilana B. Stone Dr. Janis Jermaks Dr. Samantha N. MacMillan Prof. Tristan H. Lambert 《Angewandte Chemie (International ed. in English)》2018,57(38):12494-12498
An organocatalytic oxidation platform that capitalizes on the capacity of hydrazines to undergo rapid autoxidation to diazenes is described. Commercially available benzo[c]cinnoline is shown to catalyze the oxidation of alkyl halides to aldehydes in a novel mechanistic paradigm involving nucleophilic attack, prototropic shift, and hydrolysis. The hydrolysis and reoxidation events occur readily with only adventitious oxygen and water. A survey of the scope of viable substrates is shown along with mechanistic and computational studies that give insight into this mode of catalysis. 相似文献
6.
7.
MacMillan JB Xiong-Zhou G Skepper CK Molinski TF 《The Journal of organic chemistry》2008,73(10):3699-3706
Five new cytotoxic macrolide glycosides phorbasides A-E (3-7), each possessing a macrolide ring appended to a rare ene-yne-trans-2-chlorocyclopropane, were isolated from the same Western Australian sponge (Phorbas sp.) that provided phorboxazoles A and B. The structures of 3-7 were solved by analysis of spectroscopic data including NMR, MS, and CD. A synthesis of methyl 2-O-methyl-alpha-L-evalose from L-rhamnose was completed and used for configurational assignment of the sugar residue in 3. Acid-catalyzed methanolysis of 3 followed by two-step derivatization of the liberated O-methyl glycoside gave a vicinal 4-O-naphthoyl/tertiary 3-N-(2-aminonaphthyl)carbamate derivative that exhibited exciton coupled CD identical with that of the derivative prepared from synthetic 1,2- O-dimethyl-alpha-L-evalose. 相似文献
8.
Merging Photoredox and Nickel Catalysis: The Direct Synthesis of Ketones by the Decarboxylative Arylation of α‐Oxo Acids 下载免费PDF全文
Dr. Lingling Chu Jeffrey M. Lipshultz Prof. Dr. David W. C. MacMillan 《Angewandte Chemie (International ed. in English)》2015,54(27):7929-7933
The direct decarboxylative arylation of α‐oxo acids has been achieved by synergistic visible‐light‐mediated photoredox and nickel catalysis. This method offers rapid entry to aryl and alkyl ketone architectures from simple α‐oxo acid precursors via an acyl radical intermediate. Significant substrate scope is observed with respect to both the oxo acid and arene coupling partners. This mild decarboxylative arylation can also be utilized to efficiently access medicinal agents, as demonstrated by the rapid synthesis of fenofibrate. 相似文献
9.
Anthony F. Cannella Roshaan Surendhran Samantha N. MacMillan Rupal Gupta 《Journal of Coordination Chemistry》2019,72(8):1287-1297
AbstractThis report details the synthesis and characterization of six new Mn(II) complexes coordinated to systematically varied 2,2',2''-nitrilotris(N-arylacetamidate) ligands (LR; R?=?NO2, Cl, Br, H, Me, and OMe). The complexes are synthesized as the di-tetramethylammonium salts [Me4N]2[MnLR(OAc)]. The nitro variant MnNO2 afforded crystals suitable for X-ray diffraction and its molecular structure is reported. We previously reported the crystal structures of FeNO2 and ZnNO2 and additionally report herein the synthesis and characterization of CoNO2. Using these four molecules, we conduct a brief comparison of the bond metrics to demonstrate that the primary difference governing structural changes is likely due to ionic crystal radii changes rather than electronic properties. The electrochemical properties of the MnR complexes were additionally explored with cyclic voltammetry, which revealed that the series is modulated by the various electronic substituents on the aryl groups of the ligands. The electrochemical studies also revealed, consistent with our previous report, that the acetate ligand on the MnR complexes is labile. Finally, a Hammett plot was constructed using the potentials obtained from cyclic voltammetry, which is compared with a few other similar transition metal complexes. 相似文献
10.
Vlad Bacauanu Sébastien Cardinal Motoshi Yamauchi Masaru Kondo David F. Fernández Richard Remy Prof. Dr. David W. C. MacMillan 《Angewandte Chemie (International ed. in English)》2018,57(38):12543-12548
Herein, we report a convenient and broadly applicable strategy for the difluoromethylation of aryl bromides by metallaphotoredox catalysis. Bromodifluoromethane, a simple and commercially available alkyl halide, is harnessed as an effective source of difluoromethyl radical by silyl‐radical‐mediated halogen abstraction. The merger of this fluoroalkyl electrophile activation pathway with a dual nickel/photoredox catalytic platform enables the difluoromethylation of a diverse array of aryl and heteroaryl bromides under mild conditions. The utility of this procedure is showcased in the late‐stage functionalization of several drug analogues. 相似文献