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61.
Bis- as well as tris-tetrahydropyranone ring systems were obtained via multiple tandem cyclization-1,3-dipolar cycloaddition reactions of α-diazo ketones with ketone as well as aldehyde functional groups in a chemoselective manner. 相似文献
62.
Starting from trifluoromethyl β-dicarbonyl compounds, a rare loss of CF3CO was observed in the amination reactions performed under heterogeneous conditions using NsONHCO2Et as the aminating agent and CaO or NaH as the base, while corresponding nonfluorinated β-dicarbonyl compounds under analogous conditions give non deacylated aminated compounds. This reaction can facilitate a direct synthesis of N-substituted α-amino esters or α-amino ketones. 相似文献
63.
YiHU JueCHEN ZhangGaoLE ZhenChuCHEN QinGuoZHENG 《中国化学快报》2005,16(7):903-905
An efficient method is reported for the synthesis of phenacyl esters by reaction of carboxylic acids with a-bromoacetophenone promoted by potassium fluoride in ionic liquid [Bmim]PF6, the yield of the reaction is almost quantitative and the products are essentially pure. 相似文献
64.
在SmI_2-HMPA-THF-t-BuOH体系中,硫代碳酸酯的酰硫键发生还原断裂反应,得到相应的二硫醚产物。 相似文献
65.
The introduction of quality standards for vegetable oil methyl esters is gaining in importance due to their increased use as diesel fuel substitutes and as technical products. Free and esterified sterols, the main constituents of the unsaponifiable matter in vegetable oils, are recovered in vegetable oil methyl esters and may influence the technical properties of vegetable oil methyl ester products. A rapid gas chromatographic method for the qualitative and quantitative determination of free and esterified sterols in vegetable oil methyl esters has therefore been developed. The concentration of the free sterols as well as their qualitative and quantitative composition and the concentration of the sterol esters have been determined in rape seed oil methyl ester samples by GC–FID. Prior to analysis, the free sterols were silylated with N,O-bis(trimethylsilyl)trifluoroacetamide with 1% of trimethylchlorosilane; betulinol was used as an internal standard. Calibration was performed by analysis of standard solutions containing β-sitosterol, cholesteryl stearate, and betulinol. The reproducibility of the quantitative results has been evaluated by repeated injections of the same test solution and by repeated complete analysis of the same sample. 相似文献
66.
[60]Fullerene-fused pyrazolines 1 were prepared by the reaction of C60 with alky diazoacetates under the solid-state high-speed vibration milling conditions as well as in toluene solution. Pyrazolines 1 were stable in refluxing toluene and its thermolysis process in 1,2-dichlorobenzene was investigated, the decomposition rates and activation energies of pyrazolines 1 were obtained. The current work demonstrated that the liquid-phase reaction of C60 with alkyl diazoacetates undergoes via 1,3-dipolar cycloaddition pathway at room temperature, or proceeds via carbene mechanism at a temperature of refluxing toluene, thus clarifies the previous ambiguity of its reaction mechanism. 相似文献
67.
Summary A method was devised to assay four forms of vitamin C: L-ascorbic acid (AA), dehydroascorbic acid (DHA), ascorbate-2-mono-
and polyphosphate (AMP, APP), as well as ascorbate-2-monosulphate (AMS), in sample series of different fish tissues and feed.
Direct and indirect detection were combined. Sample extractions were carried out with 0.2 mol L−1 sodium acetate buffer (pH 4.8) and extracts were deproteinized after different chemical or enzymatic reactions, with perchloric
acid. The DHA was reduced to AA with dithioerythritol (DTE). Ascorbate oxidase enzyme was used for the detection of background
and an acidic phosphatase enzyme for the hydrolysis of different phosphate esters. Ascorbate-2-sulphate was detected directly
with help of coinjection of the compound. Chromatographic analysis was carried out with a single column isocratic reverse
phase method. The mobile phase was an aqueous buffer of 0.04 M sodium-acetate, 0.05 mM EDTA, 0.5 mM tetrabutylammonium dihydrogen
phosphate (TBA) adjusted to pH 3.76 with 85% H3PO4 and with 24 mL methanol added to 1000 mL. C-18 columns were used with 0.6 mL min−1 flow rate at 23°C. The vitamin C forms were detected by UV absorption at 250 nm. The determination limit was 1.0–5.0 μg g−1 in AA equivalent. The standard deviations were between 1–6% and depended on the concentrations of vitamin C forms and tissues.
Recoveries were between 90–96% in samples.
Presented at: Balaton Symposium on High-Performance Separation Methods, Siófok, Hungary, September 3–5, 1997 相似文献
68.
X. Andrew Guo Allen D. Hunter Jie Chen 《Journal of polymer science. Part A, Polymer chemistry》1994,32(1):47-56
Five acrylic esters having different fluorine contents and distributions in their side-groups (i.e., CH2=CHC(O)OR, where R = ? C(CH3)2C6F4H, ? C(CH3)2C6F5, ? C(CF3)2C6F5, ? C(CF3)2C6H5, and ? C(CH3)2C6H5) have been prepared from the reactions of the lithium salts of their corresponding alcohols with acryloyl chloride. These monomers are polymerized under identical conditions by the radical initiator AIBN and five polyacrylates were prepared having the structure of ? [ ? CH2CHC(O)OR? ]n? . These addition polymers were compared and fully characterized by GPC, VPO, DSC, TGA, NMR, IR, and UV-visible spectroscopies, and they showed potential for practical applications. Significant differences in their thermal stabilities were found with respect to fluorine contents and distributions in these polyacrylates, and the highest stability arises from CF3 substitutions in the side-chains of the polymers. © 1994 John Wiley & Sons, Inc. 相似文献
69.
I. V. Ukrainets N. L. Bereznyakova G. P. Petyunin I. A. Tugaibei V. B. Rybakov V. V. Chernyshev A. V. Turov 《Chemistry of Heterocyclic Compounds》2007,43(6):729-739
An improved method for the preparation and purification of ethyl 2-hydroxy-4-oxo-4H-pyrido[1,2-a]-pyrimidine-3-carboxylates
is proposed. According to 1H and 13C NMR spectroscopic data the synthesized compounds exist in DMSO solution in the 2-hydroxy-4-oxo form while in the crystal
(at least for the case of the unsubstituted derivative) X-ray analysis shows that it occurs in the bipolar 2,4-dioxo form.
__________
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 864–876, June, 2007. 相似文献
70.
Yun-Yun Yang 《Tetrahedron》2006,62(43):10079-10086
A Zn(OTf)2-catalyzed cascade reaction of anilines with aromatic aldehydes and carbonyl compounds was described. This one-pot three-component reaction afforded the corresponding β-amino carbonyl compounds, β-amino esters, and β-amino ketones in good to excellent yields. The reaction was also applied for the liquid-phase synthesis of β-amino carbonyl compound library using PEG as a support. 相似文献