全文获取类型
收费全文 | 57925篇 |
免费 | 5317篇 |
国内免费 | 9557篇 |
专业分类
化学 | 53433篇 |
晶体学 | 1858篇 |
力学 | 911篇 |
综合类 | 363篇 |
数学 | 2939篇 |
物理学 | 13295篇 |
出版年
2024年 | 82篇 |
2023年 | 607篇 |
2022年 | 1344篇 |
2021年 | 1322篇 |
2020年 | 1599篇 |
2019年 | 2484篇 |
2018年 | 1528篇 |
2017年 | 2599篇 |
2016年 | 2106篇 |
2015年 | 1923篇 |
2014年 | 2557篇 |
2013年 | 4903篇 |
2012年 | 3518篇 |
2011年 | 3961篇 |
2010年 | 3105篇 |
2009年 | 3611篇 |
2008年 | 3834篇 |
2007年 | 3854篇 |
2006年 | 3620篇 |
2005年 | 3290篇 |
2004年 | 3121篇 |
2003年 | 2573篇 |
2002年 | 2272篇 |
2001年 | 1831篇 |
2000年 | 1756篇 |
1999年 | 1390篇 |
1998年 | 1195篇 |
1997年 | 1061篇 |
1996年 | 886篇 |
1995年 | 868篇 |
1994年 | 701篇 |
1993年 | 613篇 |
1992年 | 520篇 |
1991年 | 372篇 |
1990年 | 235篇 |
1989年 | 216篇 |
1988年 | 189篇 |
1987年 | 117篇 |
1986年 | 118篇 |
1985年 | 122篇 |
1984年 | 91篇 |
1983年 | 55篇 |
1982年 | 91篇 |
1981年 | 103篇 |
1980年 | 77篇 |
1979年 | 94篇 |
1978年 | 60篇 |
1977年 | 48篇 |
1976年 | 41篇 |
1974年 | 30篇 |
排序方式: 共有10000条查询结果,搜索用时 78 毫秒
991.
A. V. Kolotaev L. I. Belen’kii A. S. Kononikhin M. M. Krayushkin 《Russian Chemical Bulletin》2006,55(5):892-897
Symmetrical and unsymmetrical α-diketones of the indole series were synthesized by the Friedel-Crafts reaction of 3-indolylglyoxyl
chlorides with heterocycles. A nonconventional reaction of N-unsubstituted diketones with hydrazine producing 3H-pyrazolo[3,4-c]quinoline derivatives was found.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 862–866, May, 2006. 相似文献
992.
V. Vojinovi? 《Analytica chimica acta》2006,565(2):240-249
A new alternative method for bioprocess monitoring based on bienzymatic analytical microreactors integrated in a flow injection analysis (FIA) system is described. Glucose-, alcohol-, lactate-, galactose- and l-amino acid oxidases (GO, AO, LacO, GalO and LAAO) and horseradish peroxidase (HRP) are immobilized on controlled pore glass (CPG) and used for the development of glucose, ethanol, lactate, galactose and amino acid sensors. The analytical methodology is based on HRP catalysed reaction of hydrogen peroxide produced by oxidases with phenol-4-sulfonic acid and 4-aminoantipyrine. The immobilized enzymes are characterized and used for preparation of the packed bed analytical microreactors. Shelf life and operational stability of the microeactors are determined. GO/HRP, AO/HRP and LAAO/HRP microreactors showed excellent shelf life, they could be stored and reused for more than 6 months with no or very little activity loss, while GalO/HRP and LacO/HRP could be stored for shorter periods of time (10-20 days). Operational stability of GO and LacO microreactors was very good: an equivalent to 16,900 FIA injections of 25 μl to a LacO microreactor resulted in loss of half of its activity, immobilized GO was so stable that it was impossible to evaluate enzyme halflife. Immobilized GalO and LAAO lose their operational activity much faster: approximately 1400 and 8000 FIA injections of the respective substrate solution in a FIA set-up resulted in 50% activity loss. The methods with all the described microreactors were successfully validated using off-line samples from S. cerevisiae, E. coli and mesenchymal stem cell cultures with HPLC as the reference method. 相似文献
993.
994.
I. G. Abramov A. V. Smirnov L. S. Kalandadze N. P. Gerasimova N. A. Nozhnin V. N. Sakharov 《Chemistry of Heterocyclic Compounds》2005,41(2):238-240
New 3-aryl-substituted [1,2,4]triazolo][3,4-b][1,3]benzothiazole-6,7-dicarbonitriles have been synthesized by successive interaction of 5-aryl-4H-triazole-2-thiols with 4-bromo-5-nitrophthalonitrile in the presence of K2CO3 initially at the bromine atoms and then at the nitro group.__________Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 2, 270–272, February, 2005. 相似文献
995.
在芳烃溶剂中用氯化二乙基铝和叠氮化钠反应合成了叠氮化二乙基铝(DEAA),其产率高达87%,比文献值高出17%。在正己烷中没有合成出DEAA,在含30%四氢呋喃(THF)的正己烷中合成出DEAA·THF配合物。在芳烃溶剂中,随着苯环上甲基数目的增加,DEAA的收率增加。测定了氯化二乙基铝、氯化二乙基铝的正己烷溶液、氯化二乙基铝的甲苯溶液的 27Al NMR谱。由 27Al NMR谱数 据确定了氯化二乙基铝在甲苯中解离平衡式,计算了氯化二乙基铝在甲苯中解离平衡的热力学数据。用DEAA与苯甲酸甲酯直接合成了苯甲酰叠氮,并表征了其结构。这是一个新反应,至今无文献报导。用实验证明了在正己烷溶液中,用氯化二乙基铝、叠氮化钠与苯甲酸甲酯合成苯甲酰叠氮,没有经过氯化二乙基铝和叠氮化钠反应生成中间体DEAA的这一步。依据实验事实建立了上述三种反应的反应机理。 相似文献
996.
Heimark L Shipkova P Greene J Munayyer H Yarosh-Tomaine T DiDomenico B Hare R Pramanik BN 《Journal of mass spectrometry : JMS》2002,37(3):265-269
A liquid chromatography/mass spectrometry (LC/MS) method for separation and characterization of ergosterol biosynthetic precursors was developed to study the effect of Posaconazole on sterol biosynthesis in fungi. Ergosterol biosynthetic precursors were characterized from their electron ionization mass spectra acquired by a normal-phase chromatography, particle beam LC/MS method. Fragment ions resulting from cleavage across the D-ring and an abundant M - 15 fragment ion were diagnostic for methyl substitution at C-4 and C-14. Comparison of the sterol profile in control and treated Candida albicans incubations showed depletion of ergosterol and accumulation of C-4 and C-14 methyl-substituted sterols following treatment with Posaconazole. These C-4 and C-14 methyl sterols are known to be incapable of sustaining cell growth. The results demonstrate that Posaconazole exerts its antifungal activity by inhibition of ergosterol biosynthesis. Furthermore, Posaconazole appears to disrupt ergosterol biosynthesis by inhibition of lanosterol 14alpha-demethylase. 相似文献
997.
The applicability of (1R,2R)-1,3-diacetoxy-1-(4-nitrophenyl)-2-propyl isothiocyanate [(R,R)-DANI] as a recently developed chiral derivatizing agent for the enantioseparation of a series of β-blockers is described. The thiourea diastereomers formed were analyzed by reversed-phase high-performance liquid chromatography, mixtures of water and methanol or acetonitrile being used for elution. Conditions of derivatizations (temperature, reagent excess and reaction time) were optimized, and the effects of organic modifiers on the retention and separation were investigated; the diastereomers could readily be baseline separated with methanol-containing mobile phases with resolutions between 1.58 and 2.72. 相似文献
998.
聚羟基丁酯酯缓释微球的制备及性能 总被引:6,自引:1,他引:6
用溶剂蒸发法制备了以新型生物可降解材料聚羟基丁酸酯为载体、以安定为模药的缓释微球,讨论了药物与载体之比对药物含量与包封率的影响,以及制备微球条件对药物释放性能的影响;微球平均粒径为30~40μm,粒径分布在1~1.5之间,最大载药量为19.51%;最高包封率为67.11%;体外累积释放曲线呈“两相”释放特征并拌随初始的“突释效应”。扫描电镜观察微球表面呈皱缩表观形态结构,微球内部横断面具有孔道与孔 相似文献
999.
1000.