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31.
Antonio Alberola Rebecca J. Collis Robert J. Less Jeremy M. Rawson 《Journal of organometallic chemistry》2007,692(13):2743-2749
A general three-step synthesis to a range of benzo-fused-1,3,2-dithiazolylium salts bearing both electron-withdrawing (CN) and electron-donating (Me) groups is described. This methodology has also been extended to pyridyl derivatives and offers a potential route to a diversity of 1,3,2-dithiazolylium rings and their corresponding 1,3,2-dithiazolyl free radicals. The key steps in the reaction are treatment of a substituted 1,2,-dichlorobenzene with two equivalents of [tBuS]Na, followed by chlorination to yield the corresponding bis(sulfenyl chloride). Subsequent ring closure with Me3SiN3 yields the target 1,3,2-dithiazolylium ring system in good yield. The preparation and crystal structures of 3′-methyl-benzo-1,3,2-dithiazolylium chloride and 3′-methyl-benzo-1,3,2-dithiazolyl are described and the electronic properties of the radical examined through EPR spectroscopy, DFT calculations and variable temperature magnetic susceptibility measurements. 相似文献
32.
Four simple and sensitive spectrophotometric methods (A–D) for the determination of Ketotifen fumarate in bulk samples and pharmaceutical formulations are described. They are based on the formation of coloured species by the coupling of the diazotised sulphanilamide with the drug (method A, max 520 nm) or by oxidizing it with excessN-bromo-succinimide and determining the consumed NBS with decrease in colour intensity of celestine blue (method B: max 540 nm) or by the reduction of Folin-Ciocalteau reagent (method C: max 720 nm) or by the formation of a chloroform-soluble, coloured ionassociation complex between the drug and Azocarmine G at pH 1.5 (method D: max 540 nm). Regression analysis of Beer-Lambert plots showed good correlations in the concentration ranges 1–10, 2–12, 4–28 and 2.5–25 g/ml for methods A–D, respectively. The validity of the proposed methods was tested by analysing pharmaceutical formulations containing KTF: the relative standard deviations were within ±1.0%. Recoveries were 98.9–100.2%. 相似文献
33.
Mark J. Thompson 《Tetrahedron letters》2006,47(14):2361-2364
A convenient route to 4-phenyl-5-aminothiazoles is described, which offers control over substitution at the 2-position. 2-N-Acylglycinamides were dithionated and a subsequent TFAA-mediated cyclisation step was followed by removal of the 5-N-trifluoroacetyl group providing the free amines. Though applicable generally the method was found to be most effective when introducing aromatic substituents at the 2-position, whereupon moderate overall yields of the 5-amino compounds were obtained. 相似文献
34.
A new method for silylation of allyl ethers with chlorosilanes has been developed by the use of Cp2TiCl2 as a catalyst. This reaction proceeds efficiently at −20 °C in THF using nBuMgCl. A plausible reaction pathway via allyltitanocene intermediate was proposed. 相似文献
35.
In this work, a new ligand, 2,9-bis[N,N-bis(carboxymethyl)-aminomethyl]-1,10-phenanthroline (BBCAP), was synthesized and
used to establish a novel fluorimetric method for the determination of trace amounts of terbium in a binary system. Its luminescence
mechanism was studied. The excitation and emission wavelengths are 284 nm and 547 nm, respectively. Other rare-earth metal
ions in 100-fold excess caused no interference. The fluorescence intensity was a linear function of the concentration of terbium
in the range of 5.0 × 10−10–1.0 × 10−6 mol/L. The detection limit was 2.0 × 10−11 mol/L (n = 12). The standard addition method was used to determine the terbium in a synthetic rare-earth sample with satisfactory
results. This method represents a direct, rapid, selective and sensitive analytical procedure with a widely linear range.
Received November 29, 2001 Revision February 9, 2002 相似文献
36.
Sheng-Lou?DengEmail author Ru-Yu?Chen 《Monatshefte für Chemie / Chemical Monthly》2004,135(9):1113-1119
Summary. A new and simple method for the synthesis of 1,3,2-diazaphosphorines and 1,3,2-oxazaphosphorine was developed based on the reactions of Lawessons reagent with -aminopropionitriles and -hydroxypropionitrile. In addition, a rapid and facile synthesis of 1,3,2-diazaphospholidin-4-ones by the reaction of P(NEt2)3 with hindered diamino substrates under microwave irradiation was also achieved. The prepared phosphorines show herbicidal activity to some extent in the preliminary bioassays. 相似文献
37.
Peroxisomicine A1 is a potentially antineoplastic compound isolated from the seeds of Karwinskia parvifolia. It is considered as a useful chemotype for the preparation of topoisomerase II targeted anticancer cells. Stereochemically, it is characterized by the presence of two stereocenters and a rotationally hindered and thus likewise stereogenic biaryl axis. In this contribution, the absolute configuration of peroxisomicine A1 and its epimer, peroxisomicine A2, was established by means of a five-step degradative procedure giving the respective R- and S-configured methyl 2-(2′-methyl-5′-oxotetrahydrofuryl)acetates. The configuration of the degradation product was obtained by means of optical rotation, 1H NMR analysis using a chiral displacement reagent, and by experimental and quantum chemical circular dichroism (CD) investigations. Based on the results obtained here and considering our previous work on the relative configuration at centers versus axis of these compounds, peroxisomicine A1 resulted to be the P,3S,3′S-isomer and peroxisomicine A2 the P,3R,3′S-isomer. 相似文献
38.
本文报道了三异丙氧钐(5%)催化下,以乙酸乙酯为乙酰化试剂醇的选择性乙酰化反应。此法操作简便,产率良好。 相似文献
39.
Immobilized sulfhydryl groups were prepared by partial thiolation of NH2-glass beads. The microenvironment of the immobilized SH groups was varied by different chemical modifications of neighboring
NH2 groups. Introduction of a strong charge in the surroundings of immobilized sulfhydryls results in their dramatic stabilization
against autooxidation. This effect is due to the salting of O2 from the surface microlayer of the thiolated beads. 相似文献
40.