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1.
13C-NMR studies of marine natural products II. Total assignment of the 13C-NMR spectrum of asperdiol
13C-nmr spectral assignments for asperdiol are made with the aid of model compounds and T1 relaxation behavior. Overall isotropic tumbling was inferred from the latter providing a supplemental means of multiplicity determination. Utilization of the T1 relaxation times as an assignment criterion for select resonances in asperdiol is also described. 相似文献
2.
Shannon E. Cooney Alex A. Fertig Madeleine R. Buisch William W. Brennessel Ellen M. Matson 《Chemical science》2022,13(43):12726
Hydrogen-atom (H-atom) transfer at the surface of heterogeneous metal oxides has received significant attention owing to its relevance in energy conversion and storage processes. Here, we present the synthesis and characterization of an organofunctionalized polyoxovanadate cluster, (calix)V6O5(OH2)(OMe)8 (calix = 4-tert-butylcalix[4]arene). Through a series of equilibrium studies, we establish the BDFE(O–H)avg of the aquo ligand as 62.4 ± 0.2 kcal mol−1, indicating substantial bond weaking of water upon coordination to the cluster surface. Subsequent kinetic isotope effect studies and Eyring analysis indicate the mechanism by which the hydrogenation of organic substrates occurs proceeds through a concerted proton–electron transfer from the aquo ligand. Atomistic resolution of surface reactivity presents a novel route of hydrogenation reactivity from metal oxide surfaces through H-atom transfer from surface-bound water molecules.Coordination-induced bond weakening facilitates H-atom transfer from polyoxovanadate surface. 相似文献
3.
Lana G. Kaiser Ma?gorzata Marjańska Gerald B. Matson Isabelle Iltis Seth D. Bush Brian J. Soher Susanne Mueller Karl Young 《Journal of magnetic resonance (San Diego, Calif. : 1997)》2010,202(2):259-266
Glutathione (GSH) is a powerful antioxidant found inside different kinds of cells, including those of the central nervous system. Detection of GSH in the human brain using 1H MR spectroscopy is hindered by low concentration and spectral overlap with other metabolites. Previous MRS methods focused mainly on the detection of the cysteine residue (GSH-Cys) via editing schemes. This study focuses on the detection of the glycine residue (GSH-Gly), which is overlapped by glutamate and glutamine (Glx) under physiological pH and temperature. The first goal of the study was to obtain the spectral parameters for characterization of the GSH-Gly signal under physiological conditions. The second goal was to investigate a new method of separating GSH-Gly from Glx in vivo. The characterization of the signal was carried out by utilization of numerical simulations as well as experiments over a wide range of magnetic fields (4.0–14 T). The proposed separation scheme utilizes J-difference editing to quantify the Glx contribution to separate it from the GSH-Gly signal. The presented method retains 100% of the GSH-Gly signal. The overall increase in signal to noise ratio of the targeted resonance is calculated to yield a significant SNR improvement compared to previously used methods that target GSH-Cys residue. This allows shorter acquisition times for in vivo human clinical studies. 相似文献
4.
Iodomethyl-, chloromethyl-, and fluoromethyldimethylsulfonium salts, 4b-d, have been synthesized and are observed to be highly reactive molecules that exhibit extraordinary diversity with respect to the nature of their reactivity, undergoing facile direct substitution (S(N)2) reactions, but also being highly susceptible to electron-transfer reactions. Cyclic voltametry experiments indicated that the iodomethyldimethylsulfonium compound, 4b, is a potent electron acceptor, even surpassing the reactivity of perfluoro-n-alkyl iodides in that capacity. The iodo- and chloromethyldimethylsulfonium salts, 4b,c, as well as the analogous iodomethyltrimethylammonium salt, 3a, are shown to be reactive SET acceptors. 相似文献
5.
High-dimensional, multispectral data on complex physical systems are increasingly common. As the amount of information in data sets increases, the difficulty of effectively utilizing it also increases. For such data, summary information is required for understanding and modeling the underlying dynamics. It is here proposed to use an extension of computational mechanics [C. R. Shalizi and J. P. Crutchfield, J. Stat. Phys. 104, 817 (2001)] to arbitrary spatiotemporal and spectral dimension, for providing such summary information. An example of the use of these tools to identify state evolution in the brain, an archetypal, complex biophysical system, serves as an illustration. 相似文献
6.
Scott C. Radzinski Jeffrey C. Foster John B. Matson 《Macromolecular rapid communications》2016,37(7):616-621
Bottlebrush polymers are synthesized using a tandem ring‐opening polymerization (ROP) and ring‐opening metathesis polymerization (ROMP) strategy. For the first time, ROP and ROMP are conducted sequentially in the same pot to yield well‐defined bottlebrush polymers with molecular weights in excess of 106 Da. The first step of this process involves the synthesis of a polylactide macromonomer (MM) via ROP of d ,l ‐lactide initiated by an alcohol‐functionalized norbornene. ROMP grafting‐through is then carried out in the same pot to produce the bottlebrush polymer. The applicability of this methodology is evaluated for different MM molecular weights and bottlebrush backbone degrees of polymerization. Size‐exclusion chromatographic and 1H NMR spectroscopic analyses confirm excellent control over both polymerization steps. In addition, bottlebrush polymers are imaged using atomic force microscopy and stain‐free transmission electron microscopy on graphene oxide.
7.
Hydrolytically-labile hydrazones in peptide amphiphiles were studied as degradable tethers for release of the drug nabumetone from nanofiber gels. On-resin addition of the novel compound tri-Boc-hydrazido adipic acid to a lysine ε-amine allowed for precise placement of a hydrazide in a peptide sequence. 相似文献
8.
Nanoparticles containing fluorine-18 were prepared from block copolymers made by ring opening metathesis polymerization (ROMP). Using the fast initiating ruthenium metathesis catalyst (H2IMes)(pyr)2(Cl)2Ru=CHPh, low polydispersity amphiphilic block copolymers were prepared from a cinnamoyl-containing hydrophobic norbornene monomer and a mesyl-terminated PEG-containing hydrophilic norbornene monomer. Self-assembly into micelles and subsequent cross-linking of the micelle cores by light-activated dimerization of the cinnamoyl groups yielded stable nanoparticles. Incorporation of fluorine-18 was achieved by nucleophilic displacement of the mesylates by the radioactive fluoride ion with 31% incorporation of radioactivity. The resulting positron-emitting nanoparticles are to be used as in vivo molecular imaging agents for use in tumor imaging. 相似文献
9.
The reduction of a variety of highly functionalized N-acylated dihydropyrazoles (1) with BH3 x pyridine is described. The process through which this unexpectedly difficult reduction was discovered and developed is reported. A facile atom-efficient route to the N-acylated dihydropyrazole reduction precursors (1) is also illustrated. The resulting acylpyrazolidine products (2) that arise upon reduction were isolated in good to high yields following exposure to reaction conditions which have been shown to tolerate a variety of different functional groups. Finally, this route has been demonstrated on a kilogram scale and provides direct access to potential proline surrogates for peptidomimetic applications. 相似文献
10.