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51.
V. Slavinska Dz. Sile G. I. Chipens Yu. Balodis G. Rozenthal K. Venteris E. Lukevics 《Chemistry of Heterocyclic Compounds》2003,39(12):1579-1583
A method was developed for the synthesis of N-[1-(S)-(ethoxycarbonyl)-3-phenylpropyl]alanylproline (enalapril) by reductive alkylation of alanylproline with ethyl 2-oxo-4-phenylbutenoate under the conditions of hydrogenation in the presence of palladium black and 1.6% Pd/C. The yield of enalapril amounted to 65%. With the ethyl ester of the -oxo acid the diastereoselectivity of formation of the S,S,S-diastereomer was higher than with the saturated synthon. It is assumed that with ethyl 2-oxo-4-phenylbutenoate as synthon a conformationally restricted surface complex is formed between the unsaturated synthon and the active centers of the catalyst. During reductive alkylation of alanylproline by ethyl 2-oxo-4-(2-thienyl)butenoate poisoning of the catalyst occurs. 相似文献
52.
标题化合物C19H23O4Cl(4)是由邻氯苯甲醛(1)与5,5-二甲基-1,3-环己二酮(2)、2,2-二甲基-1,3-二氧六环-4,6-二酮(3)在乙醇中反应而得。结构通过单晶X-射线衍射分析确定,其晶体属于单斜晶系,空间群晶体结构用直接法解出,使用全矩阵最小二乘法对原子参数进行修正,最后的偏离因子R=0.034,Rw=0.042。在晶体结构中存在一个共轭的烯醇结构。单晶X-射线分析表明;平面1(C(1)~C(6)、Cl)和平面2(C(8)~C(10)、C(12)、C(13))之间的两面角为97.11°,原子C(7)呈变形的四面体构型。 相似文献
53.
A. A. Vasil'ev A. L. Vlasyuk G. V. Kryshtal E. P. Serebryakov 《Russian Chemical Bulletin》1995,44(10):1946-1951
Stereospecific syntheses of (±)-3-methyl-6-isopropenyl-3(Z),9-decadien-1-yl acetate and (±)-3,9-dimethyl-6-isopropenyl-3(Z),9-decadien-1-yl propionate (the Racemoc forms of the pheromones of the scalesAonidiella aurantii andPseudaulascaspis pentagona) with a geometrical purity of the (Z)-trisubstituted double bond not lower than 99 % were performed. The key step in both syntheses was the 1,4-cis-hydrogenation of the corresponding ethyl 3-methyl-6-(1, 1-ethylenedioxyethyl)-2,4,9-decatrienoates catalyzed with chromium carbonyl complexes. These 2,4-dienes were obtained in five conventional steps including the alkylation of ethyl acetoacetate by the appropriate 1-bromo-3-butenes and the Horner-Emmons olefination of the corresponding -branched aldehydes.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 2026–2031, October, 1995. 相似文献
54.
本文对Ln(phen)(C6H5COO)3、Ln(phen)2P-(OC6H4CHO)3·3H2O.Ln(phen)2P-(OC6H4COOC2H5)3(Ln=Tb、Eu)固体配合物的制备和光谱性质进行了研究。根据元素分析、红外光谱、摩尔电导测定,X射线粉末衍射、热重差热分析以及紫外可见光谱确定了其组成及配位形式,并对其发光性能进行了研究。 相似文献
55.
The addition of secondary and primary amines to ethyl (1-amino-9,10-anthraquinon-2-yl)propynoate affords an easily separable
mixture of the corresponding ethyl 3-dialkylaminoor 3-alkylamino-3-(1-amino-9,10-anthraquinon-2-yl)acrylate and 3-dialkylamino-
or 3-alkylaminonaphthol[2,3-h]quinoline-2(1H), 7,12-trione (in ∼4: 1 ratio). Intramolecular cyclization of the resulting substituted ethyl acrylates results in the formation
of 4-dialkylaminoor 4-alkylamino-2-chlorinated pyridine rings. Subsequent nucleophilic substitution of the chlorine atom gives
2-functionalized 4-dialkylamino- or 4-alkylaminonaphtho[2,3-h]quinoline-7,12-diones.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2327–2332, November, 1998. 相似文献
56.
《Electroanalysis》2006,18(12):1193-1201
A chemically modified carbon paste electrode with 2,7‐bis(ferrocenyl ethyl)fluoren‐9‐one (2,7‐BFEFMCPE) was employed to study the electrocatalytic oxidation of ascorbic acid in aqueous solution using cyclic voltammetry, differential pulse voltammetry and chronoamperometry. The diffusion coefficient (D=1.89×10?5 cm2 s?1), and the kinetic parameter such as the electron transfer coefficient, α (=0.42) of ascorbic acid oxidation at the surface of 2,7‐BFEFMCPE was determined using electrochemical approaches. It has been found that under an optimum condition (pH 7.00), the oxidation of ascorbic acid at the surface of such an electrode occurs at a potential about 300 mV less positive than that of an unmodified carbon paste electrode. The catalytic oxidation peak currents show a linear dependence on the ascorbic acid concentration and linear analytical curves were obtained in the ranges of 8.0×10?5 M–2.0×10?3 M and 3.1×10?5 M–3.3×10?3 M of ascorbic acid with correlation coefficients of 0.9980 and 0.9976 in cyclic voltammetry and differential pulse voltammetry, respectively. The detection limits (2δ) were determined to be 2.9×10?5 M and 9.0×10?6 M with cyclic voltammetry and differential pulse voltammetry, respectively. This method was also examined for determination of ascorbic acid in pharmaceutical preparations. 相似文献
57.
A modification of a procedure by Hage [1] is proposed for the gas chromatographic evaluation of the content of free medium-chain fatty acids and related ethyl esters in beer. The method involves extraction of free fatty acids and ethyl esters by SPE using C18 bonded phase columns, derivatization of free fatty acids and related ethyl esters with diazomethane, and GC analysis using an SP-2340 capillary column. The results obtained have shown the method to be rapid and highly reproducible. The technique has been compared with other methods used for determination of free fatty acids. 相似文献
58.
J. G. Dunn A. C. Chamberlain N. G. Fisher J. Avraamides 《Journal of Thermal Analysis and Calorimetry》1997,49(3):1399-1408
The thermal decomposition of SEX in a nitrogen atmosphere was studied by coupled thermogravimetry-Fourier transform infrared spectroscopy (TG-FTIR), and by pyrolysis-gas chromatography-mass spectrometry (py-GC-MS). The TG curve exhibited two discrete mass losses of 45.8% and 17.8% respectively, at 200 and 257–364°C. The evolved gases identified as a result of the first mass loss were carbonyl sulfide (COS), ethanol (C2H5OH), ethanethiol (C2H5SH), carbon disulfide (CS2), diethyl sulfide ((C2H5)2S), diethyl carbonate ((C2H5O)2CO), diethyl disulfide ((C2H5)2S2), and carbonothioic acid, O, S, diethyl ester ((C2H5S)(C2H5O)CO). The gases identified as a result of the second mass loss were carbonyl sulfide, ethanethiol, and carbon disulfide. Hydrogen sulfide was detected in both mass losses by py-GC-MS, but not detected by FTIR. The solid residue was sodium hydrogen sulfide (NaSH).SEX was adsorbed onto activated carbon, and heated in nitrogen. Two discrete mass losses were still observed, but in the temperature ranges 100–186°C (7.8%) and 186–279°C (11.8%). Carbonyl sulfide and carbon disulfide were now the dominant gases evolved in each of the mass losses, and the other gaseous products were relatively minor. It was demonstrated that water adsorbed on the carbon hydrolysed the xanthate to cause the first mass loss, and any unhydrolysed material decomposed to give the second mass loss.Mr. N. G. Fisher would like to thank the A. J. Parker CRC for Hydrometallurgy for the provision of a PhD scholarship. 相似文献
59.
Zhenbin Niu Xingyuan Zhang Jiabing Dai Heping Zhang 《Frontiers of Chemistry in China》2007,2(2):151-155
A new kind of ultraviolet (UV) curable waterborne polyurethane acrylate dispersion was synthesized based on hydroxyl-terminated
polybutadiene (HTPB), poly-(propylene glycol) (PPG), isophorene diisocyanate (IPDI), 2-hydroxy ethyl acrylate (HEA) and dimethylol
propionic acid (DMPA) after neutralizing by triethylamine (TEA). 2-Hydroxy-1-[4-2-hydroxyethoxy) phenyl]-2-methyl-1-propanone
(Irgacure 2959) was used as a photoinitiator and deionized water as a diluent. Fourier transform infrared (FTIR) analysis
was used to identify the chain structure of the UV-curable polyurethane prepolymer based on HTPB and the curing process. Effects
of relative content of HTPB and PPG on emulsion stability, resistance to water and ethanol, thermal stability, compatibility
of soft and hard segment, as well as the mechanical property of the cured film were investigated.
Translated from Polymer Materials Science and Engineering, 2006, 22(3): 199–203 (in Chinese) 相似文献
60.
Nickel acetate promoted reaction of diethyl acetone-1,3-dicarboxylate with N-cyanobenzamidine led to ethyl 4-amino-6-ethoxycarbonylmethyl-2-phenylpyrimidine-5-carboxylate, upon treatment of which with
RNH2, the corresponding 6-(carbamoylmethyl)pyrimidines were obtained. Cyclization of the latter upon treatment with MeONa afforded
6-R-4-amino-7-hydroxy-2-phenylpyrido[4,3-d]pyrimidin-5(6H)-ones.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2212–2214, November, 2007. 相似文献