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排序方式: 共有1338条查询结果,搜索用时 26 毫秒
21.
22.
A new and easy protocol for the formation of substituted 4,5-dihydro-1,2,4-triazin-6(1H)-ones was developed on solid support. The heterocyclic compounds were formed by nucleophilic reaction of hydrazine on thioamide esters. As cyclization was concomitant with cleavage from the support, substituted 4,5-dihydrotriazinones were obtained in high purity. 相似文献
23.
François-Hugues PoréeAlexandre Clavel Jean-François Betzer Ange PancraziJanick Ardisson 《Tetrahedron letters》2003,44(40):7553-7556
A (Z)-vinyl (N,N-diisopropyl)carbamate treated with Grignard reagents, under Wenkert Nickel-catalysed conditions, gave access to several substituted (Z)-alkenyl derivatives. These Nickel-catalysed reactions, carried out with vinyl-, phenyl-, p-methoxyphenyl-, trimethylsilylmethylmagnesium bromide and benzylmagnesium chloride, led to the corresponding (Z)-alkenyl derivatives in good yields and high stereoselectivities. 相似文献
24.
A novel Mitsunobu-based protocol has been developed for the synthesis of O,S-dialkyl dithiocarbonates from a variety of primary, secondary and tertiary alcohols using carbon disulfide, in good to excellent yields. This protocol is mild and efficient compared to other reported methods. 相似文献
25.
The treatment of 3,4-dihydropyrimidin-2-ones with n-BuLi at −78 °C, followed by quenching with various electrophiles furnished N3-substituted derivatives, regioselectively. Further, N1,N3-diacyl derivatives were found to transfer N1-acyl groups to nucleophilic sites. 相似文献
26.
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
27.
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
28.
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
29.
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
30.
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