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71.
Kadota I Takamura H Sato K Ohno A Matsuda K Satake M Yamamoto Y 《Journal of the American Chemical Society》2003,125(39):11893-11899
The convergent total syntheses of gambierol (1) and 16-epi-gambierol (2) have been achieved. The ABC and FGH ring segments 4 and 5 were prepared from known compounds 6 and 13, respectively, by linear manners. The fragments prepared were connected by our own synthetic strategy including the intramolecular allylation of alpha-acetoxy ether followed by ring-closing metathesis to furnish the octacyclic ether 3. The diiodoalkene 45, prepared from 3, was converted to the Z-iodoalkene 50 via a novel and stereoselective hydrogenolysis followed by deprotection. Construction of the triene side chain was performed by the modified Stille coupling of 50 with the Z-vinylic stannane 41 to afford 1. The similar transformations were carried out on the epimeric octacycle 34 to give 2, which showed no toxicity against mice at the concentration of 14 mg/kg. 相似文献
72.
73.
Keisuke Nakanishi Dr. Hiroyoshi Ohtsu Prof. Dr. Gaku Fukuhara Prof. Dr. Masaki Kawano 《Chemistry (Weinheim an der Bergstrasse, Germany)》2019,25(66):15182-15188
An anionic π molecule can form an aggregate when a multi-interactivity is introduced, in sharp contrast to common anionic molecules that are generally difficult to stack on each other. We found that a multi-interactive ligand, 2,5,8-tri(4′-pyridyl)-1,3,4,6,7,9-hexaazaphenalenate (TPHAP−) exhibited a large Stokes shift and an intramolecular charge transfer, both of which were sensitive to hydrogen-bonding media. An anionic potassium salt of TPHAP− in methanol formed various aggregation states depending on the concentration examined; this was revealed by steady-state spectroscopic and fluorescence lifetime measurements. Self-assembling cadmium ions and the ligands can create several morphological crystals that are controlled by the ligand concentration, among which three new structures were determined by single-crystal analysis. The X-ray structures obtained suggest that the aggregation states of the ligand in solution can be transferred to the solid system of the porous coordination networks. 相似文献
74.
75.
Masafumi Kashii Yoichiroh Hosokawa Hiroshi Kitano Yusuke Mori Kazufumi Takano Hiroyoshi Matsumura Tsuyoshi Inoue Satoshi Murakami Kazuomi Sugamoto Takatomo Sasaki Hiroshi Masuhara 《Applied Surface Science》2007,253(15):6447-6450
For precise X-ray diffraction (XRD) measurement giving the three-dimensional structure of proteins, it is important to prepare high-quality single crystals with suitable shape. As a new processing technique to obtain such protein crystals, we employed femtosecond laser-induced cleaving of protein crystal in a growth vessel containing water solution. An intact protein crystal was precisely processed without mechanical contact in its sealed growth vessel by focusing femtosecond laser pulses. We confirmed that three-dimensional processing of the crystal in its supersaturated solution was realized using multiphoton absorption and that the processing was efficiently enhanced by the cleaving behavior attributed to a photomechanical mechanism of the femtosecond laser ablation. 相似文献
76.
Taizen Den Dr. Pavel M. Usov Dr. Jaejun Kim Dr. Daisuke Hashizume Dr. Hiroyoshi Ohtsu Prof. Dr. Masaki Kawano 《Chemistry (Weinheim an der Bergstrasse, Germany)》2019,25(49):11512-11520
Formation of coordination networks is a complex process affected by a multitude of factors. Many synthetic strategies have been developed that attempt to control these factors and direct the structure of the final product. Coordination bond formation and structural assembly processes, however, typically take place either in the solution or solid states. In comparison, gas-phase network synthesis remains largely unexplored. Herein, two new two-dimensional coordination networks are obtained from the solid–gas phase reaction between ZnX2 (X=I, Br) and the redox-active 2,5,8-tri(4-pyridyl)1,3-diazaphenalene (HTPDAP) ligand. Their structures were solved by ab initio powder X-ray diffraction analysis and feature a novel Zn halide trimeric cluster. This strategy is contrasted with a conventional solvothermal synthesis, which led to a one-dimensional coordination polymer instead. The intrinsic electroactive properties of these materials were probed by solid-state cyclic voltammetry measurements, which revealed the presence of HTPDAP and halide-based processes. Chemical oxidation of the two-dimensional networks by using NOPF6 agent, unexpectedly, led to the formation of a nitrated analog of HTPDAP, the PF6− salt of diprotonated 4,6,7,9-tetranitro-2,5,8-tris(4-pyridyl)diazaphenalene cation (denoted N-TPDAP), which was isolated and characterized. These results provide deeper insights into the oxidation process of HTPDAP-containing networks and uncover unique redox-induced chemical transformations. 相似文献
77.
Mihoko Maruyama Noriko Shimizu Shigeru Sugiyama Yoshinori Takahashi Hiroaki Adachi Kazufumi Takano Satoshi Murakami Tsuyoshi Inoue Hiroyoshi Matsumura Yusuke Mori 《Journal of Crystal Growth》2010,312(19):2771-2774
Silicone glue (modified silicone polymer) is widely used for both experiments involving inorganic crystal growth and those involving organic materials like proteins. This material is very useful for building a hand-made experiment setup or for fixing protein crystals to specific locations. Though silicone glue is regarded as harmful to proteins, no systematic verification was performed to investigate its impurity effects on protein crystal growth. We focused on and estimated the impurity effects of silicone glue on protein crystal growth. 相似文献
78.
Fujiwara M Terashima S Endo Y Shiokawa K Ohue H 《Chemical communications (Cambridge, England)》2006,(44):4635-4637
A molecular gate attached on the pore outlet of a mesoporous material, which is opened and closed by redox system of thiol groups, effectively switched the progress of a catalytic reaction promoted by the acidic site in the pore void. 相似文献
79.
Hiroyoshi Takamura Takayuki Kishi Yuichi Nakamura Yoshinori Yamamoto 《Tetrahedron》2010,66(29):5329-5344
The convergent total synthesis of brevenal, a non-toxic brevetoxin antagonist, has been achieved. The ABC ring segment and the E ring precursor were connected by the intramolecular allylation followed by ring-closing metathesis to furnish the pentacyclic ether compound. An alternative route to the key synthetic intermediate, a pentacyclic ether core, was also examined. The right- and left-hand side chains were introduced by Wittig and Horner-Wadsworth-Emmons reactions, respectively, to furnish brevenal (1). 相似文献
80.
The C14-C24 fragment of symbiodinolide possessing the 17R/18R/21R absolute configuration, which was obtained as one of the degraded products of symbiodinolide, and its diastereomer possessing the 17R/18S/21R absolute stereochemistry were synthesized stereoselectively from cis-2-butene-1,4-diol, respectively. The detailed comparison of the synthetic products with the degraded product in the spectroscopic data confirmed unambiguously that the stereostructure of the C14-C24 fragment was 17R, 18R, and 21R. 相似文献