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91.
Sekino E Kumamoto T Tanaka T Ikeda T Ishikawa T 《The Journal of organic chemistry》2004,69(8):2760-2767
(-)-Quinine-catalyzed intramolecular oxo-Michael addition (IMA) of 7-hydroxy-5-methoxy-8-tigloylcoumarins was developed for the enantioselective construction of 2,3-dimethyl-4-chromanone systems in the context of the asymmetric synthesis of anti-HIV-1 active Calophyllum coumarins. Combination of the IMA and MgI(2)-assisted demethylation of the 5-methoxy group along with isomerization of the formed chromanone systems as key steps successfully led to the concise synthesis of (+)-inophyllum B and (+)-calanolide A, possible candidates for AIDS drugs. Further examination of the asymmetric IMA with cinchona alkaloids lacking a methoxy group on the quinoline skeleton suggested the influence of the methoxy substituent on stereoselectivity at the stereogenic centers of the chromanone systems. 相似文献
92.
Takashima H Mimura N Ohkubo T Yoshida T Tamaoki H Kobayashi Y 《Journal of the American Chemical Society》2004,126(14):4504-4505
Distributed computing has been implemented to the solution structure determination of endothelin-1 to evaluate efficiency of the method for NMR constraint-based structure calculations. A key target of the investigation was determination of the C-terminal folding of the peptide, which had been dispersed in previous studies of NMR, despite its pharmacological significances. With use of tens of thousands of random initial structures to explore the conformational space comprehensively, we determined high-resolution structures with good convergences of C-terminal as well as previously defined N-terminal structures. The previous studies had missed the C-terminal convergence because of initial structure dependencies trapped in localized folding of the N-terminal region, which are strongly constricted by two disulfide bonds. 相似文献
93.
Hosoya K Hira N Watabe Y Tanaka N Kubo T Kaya K 《Analytical and bioanalytical chemistry》2004,380(2):343-345
Thiacalix[4]arene (5,11,17,23-tetra-tert-butyl-25,26,27,28-tetrahydroxy-2,8,14,20-tetrathiacalix[4]arene) is an amphiphilic molecule comprising four p-tert-butylphenol-like groups ortho-linked by single sulfur atoms. This molecule has a high electron density area owing to the close proximity of the hydroxyl groups and sulfur atoms. We studied the applicability of this interesting compound as a selector for high-performance liquid chromatography (HPLC) thereby presumably exploiting this feature. Firstly, uniformly sized polymer particles were prepared by using a multi-step swelling and polymerization method with ethylene glycol dimethacrylate (EDMA) as a cross-linker. Methacrylic acid (MAA) was introduced onto the surface of the resulting polymer particles through a new modification method. Thiacalix[4]arene was chemically bonded through the MAA group by using 1,4-dibromobutane as a spacer to reduce steric hindrance around the MAA and the polymer particle itself. The performance of the prepared polymer-based thiacalix[4]arene-modified stationary phase was evaluated with HPLC. Specific chromatographic retention behavior was observed for catechol relative to positional isomers of xylene, cresol, and benzene-diol. Catecholamine and catechol showed specific chromatographic retention behavior. 相似文献
94.
Takuya Hashimoto 《Tetrahedron letters》2010,51(4):761-8145
FeCl3/AgOTf-catalyzed hydroarylation of propiolic acid with electron-rich arenes such as mesitylene, tetramethylbenzene, and pentamethylbenzene in trifluoroacetic acid proceeded to give 3-arylpropenoic acids in moderate to high yields. The same reactions with anisole and 1,4-dimethoxybenzene afforded double hydroarylation products, 3,3-diarylpropionic acids. 相似文献
95.
Satoshi Motodate Takuya Kobayashi Mikio Fujii Prof. Tomoyuki Mochida Dr. Taichi Kusakabe Shigeki Katoh Prof. Hiroyuki Akita Prof. Keisuke Kato 《化学:亚洲杂志》2010,5(10):2221-2230
Bis(oxazoline)‐palladium(II) catalyzed carbonylation of homopropargyl alcohols afforded acyclic methoxyacrylate 2 and 6‐membered lactone 3a , 3b , 3d , 3e , 3f , 3g , 3h , 3i , 3j , 3k in good combined yield. In the case of propargyl alcohols, 5‐membered lactones 3p , 3q , 16 were obtained in moderate yields. The one‐pot synthesis of kawa lactones 3a , 3r , 3s and formal synthesis of dihydroxycystothiazole A and dihydroxycystothiazole C are presented. To elucidate the stereochemistry of (+)‐annularin G and (?)‐annularin H, the first asymmetric syntheses of these natural products were achieved. 相似文献
96.
97.
Recyclable ionic Brönsted acid was prepared in nearly quantitative yield by reacting 1-butylimidazole with an equimolar amount of 1,3-propanesultone, followed by treatment with an equimolar amount of trifluoromethanesulfonic acid. The ionic Brönsted acid-catalyzed direct benzylation, allylation and propargylation of 1,3-dicarbonyl compounds with various alcohols in ionic liquid [N-ethyl-N-methyl imidazolium trifluoromethanesulfonate (EMIOTf)], at 100 °C for 3 h proceeded smoothly to give the corresponding products in good to excellent yields without the use of any hazardous or volatile solvents and without any by-product such as salts. Furthermore, tandem benzylation-cyclization-dehydration of 1,3-dicarbonyl compounds to give functionalized 4H-chromenes was also achieved in this catalytic reaction. 相似文献
98.
The Stille cross-coupling reaction of [1-11C]acetyl chloride with tributylphenylstannane leading to [carbonyl-11C]acetophenone was studied with the goal of developing a new 11C-labeling method for positron emission tomography tracer synthesis. The coupled product [carbonyl-11C]acetophenone was synthesized using the Pd2(dba)3/P(MeNCH2CH2)3N·HCl system with a 60-61% radiochemical conversion from [1-11C]acetyl chloride (decay-corrected, n = 3). 相似文献
99.
Ken Hosoya Tomoko Mori Mari Sakamoto Takuya Kubo Kunimitsu Kaya 《Chromatographia》2009,70(5-6):699-704
We report the chromatographic properties of a new type of epoxy polymer-based monolithic capillary column, the Tetrad-C column. The column was prepared by a completely new method—reaction of a tetra-functional epoxy monomer, 1,3-bis(N,N-diglycidylaminomethyl)cyclohexane (trade name Tetrad-C), with a diamine, 4-[(4-aminocyclohexyl)methyl)cyclohexane (BACM). This polymer monolith has no aromatic functional groups reducing chromatographic performance. The columns were carefully observed by scanning electron microscopy and evaluated chromatographically by use of a μ-HPLC system. It was found that morphological control of the epoxy polymer-based monolith was possible simply by changing the polymerization conditions, i.e., the polymerization temperature and/or the relative amounts of porogenic solvent and BACM. Another advantage was that volumetric shrinkage of the tetra-functional epoxy-based monolith during the polymerization reaction was much less than for the tri-functional epoxy-based monolithic (TEPIC) column reported in our previous paper. A Tetrad-C column 200 mm long afforded up to 10,000 plates for alkylbenzenes in reversed-phase-mode. This column can also work in HILIC mode, although the hydrophobicity of the column was greater than that of the TEPIC column. Heat treatment (160 °C for 2 h; to eliminate residual, unreacted, functional groups) had a negligible effect on column performance, indicating the columns were thermally stable. 相似文献
100.
Mitsuru Suda Takuya Hagihara Noriyoshi Suya Tsuyoshi Hamano Masashi Takada Teruaki Konishi Takeshi Maeda Yasushi Ohmachi Shizuko Kakinuma Kentaro Ariyoshi Yoshiya Shimada Hitoshi Imaseki 《Radiation Physics and Chemistry》2009,78(12):1216-1219
We developed a neutron irradiation facility, neutron exposure accelerator system for biological effect experiments (NASBEE) for biological studies in National Institute of Radiological Sciences, Japan. Irradiation field of 2 MeV average neutrons generated by a Be(d–n)B reaction is established. Dose uniformity of 240 mm in diameter irradiation field is producible within ±2.5% with a dose rate of 0.87 Gy/h at sample target distance of 1170 mm. Two irradiation rooms, a specific pathogen-free (SPF) conditioned one and a conventional, are now available. Irradiation protocols for in vitro experiments are now established and demonstrated by obtaining a relative biological effectiveness (RBE) of cell inactivation measured to be 3.54 with 10% survival dose (D10). 相似文献