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Armstrong TA Bettoni D Bharadwaj V Biino C Borreani G Broemmelsiek D Buzzo A Calabrese R Ceccucci A Cester R Church MD Dalpiaz P Dalpiaz PF Dibenedetto R Dimitroyannis D Fabbri MG Fast JE Gianoli A Ginsburg CM Gollwitzer KE Hahn AA Hasan MA Hsueh SY Lewis RA Luppi E Macrí M Majewska A Mandelkern MA Marchetto F Marinelli M Marques JL Marsh W Martini M Masuzawa M Menichetti E Migliori A Mussa R Palestini S Pallavicini M Passaggio S Pastrone N Patrignani C Peoples J Pesando L Petrucci F Pia MG 《Physical review D: Particles and fields》1993,47(3):772-783
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Relatively few cyclic peptides have reached the pharmaceutical marketplace during the past decade, most produced through fermentation rather than made synthetically. Generally, this class of compounds is synthesized for research purposes on milligram scales by solid-phase methods, but if the potential of macrocyclic peptidomimetics is to be realized, low-cost larger scale solution-phase syntheses need to be devised and optimized to provide sufficient quantities for preclinical, clinical, and commercial uses. Here, we describe a cheap, medium-scale, solution-phase synthesis of the first reported highly potent, selective, and orally active antagonist of the human C5a receptor. This compound, Ac-Phe[Orn-Pro-d-Cha-Trp-Arg], known as 3D53, is a macrocyclic peptidomimetic of the human plasma protein C5a and displays excellent antiinflammatory activity in numerous animal models of human disease. In a convergent approach, two tripeptide fragments Ac-Phe-Orn(Boc)-Pro-OH and H-d-Cha-Trp(For)-Arg-OEt were first prepared by high-yielding solution-phase couplings using a mixed anhydride method before coupling them to give a linear hexapeptide which, after deprotection, was obtained in 38% overall yield from the commercially available amino acids. Cyclization in solution using BOP reagent gave the antagonist in 33% yield (13% overall) after HPLC purification. Significant features of the synthesis were that the Arg side chain was left unprotected throughout, the component Boc-d-Cha-OH was obtained very efficiently via hydrogenation of d-Phe with PtO(2) in TFA/water, the tripeptides were coupled at the Pro-Cha junction to minimize racemization via the oxazolone pathway, and the entire synthesis was carried out without purification of any intermediates. The target cyclic product was purified (>97%) by reversed-phase HPLC. This convergent synthesis with minimal use of protecting groups allowed batches of 50-100 g to be prepared efficiently in high yield using standard laboratory equipment. This type of procedure should be useful for making even larger quantities of this and other macrocyclic peptidomimetic drugs. 相似文献
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The self-assembly of unsymmetrical metal ligands from simpler components circumvents complex synthetic approaches. We show herein how a recently developed three-component assembly to create tripicolylamine-like ligands can be extended to the use of azides rather than pyridines. Substituent effects, metal dependence, and reversibility of the assembly are explored. Further, we show that the extent of assembly directly correlates with the differential binding of the templating metals between dipicolylamine-like and tripicolyamine-like ligands. 相似文献
188.
Optimised form of acceleration correction algorithm within SPH-based simulations of impact mechanics
In the context of SPH-based simulations of impact dynamics, an optimised and automated form of the acceleration correction algorithm (Shaw and Reid, 2009a) is developed so as to remove spurious high frequency oscillations in computed responses whilst retaining the stabilizing characteristics of the artificial viscosity in the presence of shocks and layers with sharp gradients. A rational framework for an insightful characterisation of the erstwhile acceleration correction method is first set up. This is followed by the proposal of an optimised version of the method, wherein the strength of the correction term in the momentum balance and energy equations is optimised. For the first time, this leads to an automated procedure to arrive at the artificial viscosity term. In particular, this is achieved by taking a spatially varying response-dependent support size for the kernel function through which the correction term is computed. The optimum value of the support size is deduced by minimising the (spatially localised) total variation of the high oscillation in the acceleration term with respect to its (local) mean. The derivation of the method, its advantages over the heuristic method and issues related to its numerical implementation are discussed in detail. 相似文献
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We prove that certain hyperbolic Coxeter groups are separable on their geometrically finite subgroups. 相似文献