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61.
3,3′:4′,3″-Ter-1,2,5-thiadiazole, an useful oligoheterocyclic compound, has been accomplished in seven steps from 1-(5-methyl-3-isoxazolyl)ethanone or diethyl acetylenedicarboxylate using a synthetic utility of tetrasulfur tetranitride antimony pentachloride (S4N4·SbCl5) complex to make a 1,2,5-thiadiazole ring. 相似文献
62.
Helmut Pfitzner und Helmut Schweppe 《Fresenius' Journal of Analytical Chemistry》1974,268(5):337-342
Zusammenfassung In einer früheren Veröffentlichung [4] ist auf die Möglichkeit der chromatographischen Trennung strukturisomerer Metallchelate hingewiesen worden; sie soll hier ausführlicher dargestellt werden. Weiterhin wird die Trennung von 1:2-Mischkomplexen von Azofarbstoffen und von 1:2-Metallkomplex-Mischungen durch Dünnschicht-Chromatographie (DC) an Polyamid beschrieben. Unter bestimmten Voraussetzungen kann durch DC an Kieselgel zwischen 1:2-Metallkomplexfarbstoffen mit Sulfonsäureamid- bzw. Alkylsulfongruppen und solchen ohne diese Substituenten unterschieden werden. Die beschriebenen DC-Methoden ermöglichen bei richtiger Interpretation eine eindeutige Unterscheidung zwischen strukturisomeren Metallkomplexen der 1:1- und 1:2-Reihe, sowie Mischkomplexen und Komplexmischungen vom 1:2-Metall-chelattyp unsulfierter o,o-Dihydroxyazoverbindungen.Symmetrische o,o-Dihydroxyazoverbindungen, wie z.B. das 2,2-Dihydroxy-5,5-dimethyl-azobenzol(7), sind geeignete Komplexbildner für Schwermetallkationen, um diese als farbige Chelate mit Hilfe der DC voneinander zu trennen. Strukturisomere sind wegen der Molekülsymmetrie ausgeschlossen, so daß die Ergebnisse eindeutig sind.
1:1 and 1:2 metal chelates of unsulphonated o,o-dihydroxyazo compounds: A thin-layer chromatographic investigation
In an earlier publication [4] the possibility of the Chromatographic separation of structurally isomeric metal chelates was mentioned; this is dealt with here in more detail. Further the separation of 1:2 mixed complexes from azo dyes and 1:2 metal-complex mixtures by thin-layer chromatography (TLC) on polyamide is described. In certain circumstances it is possible to distinguish between 1:2 metal-complex dyes with sulphonamide or alkylsulphonyl groups and those without these substituents by TLC on silica gel. The TCL methods described allow-when correctly interpreted-an unambiguous distinction between structurally isomeric metal complexes of the 1:1 and 1:2 series, and mixed complexes and mixtures of complexes of the 1:2 metal-chelate type of unsulphonated o,o-dihydroxyazo compounds.Symmetrical o,o-dihydroxyazo compounds, such as 2,2-dihydroxy-5,5-dimethylazobenzene(7), are suitable as complex-formers for heavy-metal ions, allowing the separation of the latter as their coloured chelates with aid of TLC. Structural isomers are excluded because of the molecular symmetry, so that the results are unambiguous.相似文献
63.
The initial formation of organotin derivatives with Sn-S-N bonds in heterolytic reactions of hexamethylditin or trimethyltin sulfide withN-(chlorothio)phthalimide is suggested. Subsequent interaction of these compounds with sulfenyl chloride affordsN, N-thioorN, N-dithiobisphthalimide. Homolytic reaction of hexamethylditin withN, N-dithiobisphthalimide also occursvia an organotin intermediate, which, in the absence of a nucleophilic reagent, eliminates sulfur and converts intoN-trimethylstannylphthalimide.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2111–2114, December, 1993. 相似文献
64.
Sevim Akyüz Tanil Akyüz J. Eric D. Davies 《Journal of inclusion phenomena and macrocyclic chemistry》1993,15(2):105-119
The adsorption of 4,4-bipyridyl by natural sepiolite and smectite group clay minerals (bentonite, hectorite and saponite) from Anatolia (Turkey) has been studied using vibrational spectroscopy. Investigation of Fourier-transform infrared and Fourier-transform Raman spectra of adsorbed 4,4-bipyridyl indicate the presence of chemisorbed species. However, any evidence for the generation of anionic species on the surface of the phyllosilicates has not been detected. It is proposed that the adsorbed bipyridyl molecules on sepiolite are centrosymmetric and H-bonded to the surface hydroxyls through both the nitrogen lone pairs as bidentate ligands. The adsorbed bipyridyl molecules on the smectite group clays are coordinated to exchangeable cations both directly and also indirectly through water as monodentate ligands. XRD patterns of the clays studied are also recorded. 相似文献
65.
I. I. Ponomarev Yu. Yu. Rybkin E. I. Goryunov P. V. Petrovskii K. A. Lyssenko 《Russian Chemical Bulletin》2004,53(12):2881-2883
The reaction of 4,4-dimethyldiphenyl ether with phosphorus trichloride in the presence of anhydrous aluminum chloride was studied. This reaction affords 2,8-dimethyl-10H-105-phenoxaphosphine 10-oxide as virtually the only product. In air, the latter in an alkaline solution is quantitatively transformed into 10-hydroxy-2,8-dimethyl-10H-105-phenoxaphosphine 10-oxide.__________Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2762–2765, December, 2004. 相似文献
66.
Lanying?Yang Yi?Zhang Qingqi?Chen Jin Shi?MaEmail author 《Monatshefte für Chemie / Chemical Monthly》2004,135(2):223-229
Summary. 1-(Dipyrrin-2-yl)-1-(dipyrrin-3-yl)methane, the N-confused analog of biladiene-ac, is prepared by condensation of 2,3-dipyrromethane with two molecules of 2-formylpyrrole in dichloromethane in the presence of hydrogen bromide. Self-assembly of the ligand with Zn(II) in dichloromethane and methanol offers a dinuclear dimeric complex with a ligand:metal ratio of 2:2. X-Ray crystal structure analysis reveals two ligands bound through a head-to-tail pattern to two zinc centers to form a severely distorted helical conformation, which has the shape of a rectangle. 相似文献
67.
Šárka Králíková 《Tetrahedron》2006,62(20):4917-4932
We found that various dialkyl phosphites, dialkyl trimethylsilyl phosphites, and tris-trimethylsilyl phosphite reacted smoothly with nucleoside 5′-aldehydes to afford epimeric nucleoside 5′-C-phosphonates in high yields. A number of these compounds in both the 2′-deoxyribo and ribo series were prepared. In the case of 2′-deoxythymidine-5′-aldehyde, a thorough study was made on the influence of the 3′-hydroxyl protecting group, type of phosphite, base, and solvent, on the yield and epimeric ratio of the resulting 5′-hydroxyphosphonates. Partial stereoselectivity in favour of either R or S epimers was observed. An attempt to transform the α-hydroxyl of the phosphonate moiety into a halo or azido moiety was not successful. Only intramolecular substitution reaction of the mesyloxy group for an alkoxy residue of the 2-hydroxyethyl ester took place in a low yield. 相似文献
68.
S. G. Zlotin M. V. Sharashkina Yu. A. Strelenko O. A. Luk'yanov M. O. Dekaprilevich Yu. T. Struchkav 《Russian Chemical Bulletin》1994,43(7):1220-1226
Methods for the synthesis of polyfunctionalN-phosphoryl- andN-phosphonoyldiazeneN-oxides containing hydroxyl, acetoxyl, and nitrate groups, and dibromoallyl and dibromopropyl fragments have been developed. The molecular structure ofN-(2,2-dimethyl-5-nitro-1,3-dioxan-5-yl)-N-[methoxy(phenyl)phosphoryl)diazeneN-oxide was established by X-ray structural analysis.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1284–1289, July, 1994. 相似文献
69.
Michael Leuck Rubina Giare Matthias Paul Nicole Zien Andreas Wolter 《Tetrahedron letters》2004,45(2):317-320
A novel improved controlled pore glass (CPG) support based on the 2-(hydroxymethyl)-6-nitrobenzoyl (HMNB) protecting group was developed for the synthesis of 3′-aminoalkylated oligonucleotides. The release of oligonucleotides with free 3′-amino groups from the support is complete within 2 h at 55 °C in concentrated ammonia. 相似文献
70.
Electropolymerization of 3,3′-diaminobenzidine on a gold surface gave an adherent, stable film of poly(3,3′-diaminobenzidine) (PDAB). This polymer film retained the complexational functionalities of its monomer, demonstrating preconcentration abilities for several ions, including Se(IV) and Te(IV). In particular, in this work, continuous flow and flow injection methods were developed for the sensitive and selective determination of Te(IV). The optimized method for the continuous flow mode had a detection limit of 5.6×10−9 mol l−1 for 10 min preconcentration. Typical relative standard deviations for six consecutive determinations were 1.82 and 2.56% for Te(IV) concentrations of 1.0×10−6 and 5.0×10−8 mol l−1, respectively (10 min preconcentration). The method was applied to the determination of Te(IV) in real samples. 相似文献