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991.
A new method for the preparation of the synthon (±)-2,6,7,7a-tetrahydro-1β-hydroxy-4-formyl-7aβ-methylindene (1,a) for the
total synthesis of steroids in both (±) and (+) forms, starting from the known β-ketoester, (±)-methyl 1β-t-butoxy-5,6,7,7a-tetrahydro-7aβ-methyl-5-keto-4-indancarboxylate (2,a) has been described. An alternative route to (1,a) has
been investigated. Although the compound, (±)-1β-hydroxy-5,6,7,7a-tetrahydro-7aβ-methyl-5-keto-4-methoxymethylindan (2,b)
could not be prepared, interesting pathways leading to two unexpected products, (±)-5,6,7,7a-tetrahydro-4,7a-dimethyl-5H-indene-1,5-dione
and (±)-2,6-diketo-3-methyltricyclo-(5,2,1,0)decan-8-ol (3 and 4), were encountered during an attempted annelation reaction
of the ketone, N-diethylamino-5-methoxypentan-3-one (6), with 2-methylcyclopentan-1,3-dione (5). Trapping of the intermediate,
(±)-3a,4,5,6,7,7a-hexahydro-3a-hydroxy-4-methylene-7a-methylindene-1,5-dione (7), through the formation of the adduct, (±)-3a,4,5,6,7,7a-hexahydro-3a-hydroxy-4-(1′,
3′-diketo-2′-methylcyclopentano-2′-methylene)-7a-methylindene-1,5-dione (8), established the mechanism of the formation of
the products (3 and 4). 相似文献
992.
In our former investigations, the phenomenon high temperature corrosion (HTC) was described exemplarily on selected materialcoating combinations for blades of stationary gas turbines, mainly in the temperature region of up to 750° C. To answer the question, in which manner higher gas inlet and/or higher material surface temperature would influence the HTC behaviour, a special analytical technique—the integral layer profile analysis—was introduced to ameliorate concentration profile methods. By examining IN 738 LC specimens with CoCrAlY plasma spray coating, stressed by hot gas at 900° C, the limits of this system are shown by explaining the corrosion mechanism; the method is also used for other systems, e.g. U 520 with NiCrAlY coating at 750° C. 相似文献
993.
Rashid A. Zeineh George Kyriakidis Roger Acey Christopher Smith 《Applied biochemistry and biotechnology》1986,13(2):119-125
Citrus tristeza virus (CTV) extracted from Etrog citron (C.medica L.) was immunoprecipitated. The immunoprecipitate was fractionated by SDS-PAGE and western blotted onto nitrocellulose. The CTV
antigens were determined by immunoblot analysis using rabbit anti-CTV IgG, and the protein-band pattern exhibited on the nitrocellulose
was assessed by soft-laser scanning densitometry. The densitometric tracing revealed the presence of bands that were not visible
to the naked eye. Using the superimposition mode of the instrument, it was also revealed that the protein-band patterns of
different CTV samples were not identical. Computer-aided soft-laser scanning densitometry proved to be a powerful approach
in the detection and assessment of protein bands revealed on nitrocellulose immunoblots, which we were previously unable to
do employing conventional methods. 相似文献
994.
The product distributions from bifunctional conversion ofn-decane over Pt/SAPO-5 and Pt/SAPO-11 catalysts are compared in detail. Selectivities in decane reaction vary largely with
the catalyst employed: Pt/SAPO-11 produces high yields of feed isomers, whereas Pt/SAPO-5 gives high yields of cracked products
and only under mild reaction conditions are isodecanes the main products obtained. These selectivities seem to be determined
by the structure of the catalyst. 相似文献
995.
3-O-Acetyl-1,2-O-isopropylidene--D-allofuranose (2 b) was prepared from 1,2:5,6-di-O-isopropylidene--D-allofuranose (1 b). Treatment of2 b with triphenylphosphine-diethyl azodicarboxylate afforded regio- and stereospecifically the 5,6-epoxy--D-allo derivative (3). The other diastereomeric compound, 5,6-epoxy-1,2-O-isopropylidene--L-talofuranose (6) was also prepared stereoselectively from2 b
via the intermediates5 a and5 b. The epoxy sugars3 and6 were converted with lithium aluminum hydride to the corresponding 6-deoxy-1,2-O-isopropylidene--D-allofuranose (4 a) and --L-talofuranose (7 a) derivatives. Hydrolysis of4 a and7 a afforded 6-deoxy-D-allose and 6-deoxy-L-talose, respectively. The corresponding 3,5-di-O-acetyl- (4 b and7 b) and the 3,5-O-(tetraisopropyldisiloxane-1,3-diyl) derivatives (4 c and7 c) are also described. Selective removal of the isopropylidene group and subsequent acetylation offers a convenient route to prepare sugar derivatives containing furanose ring, like8 b, as a suitable precursor for nucleoside analogs.Herrn Prof. Dr.K. Komarek mit den besten Wünschen zum 60. Geburtstag gewidmet. 相似文献
996.
N. Ya. Grigorieva 《Russian Chemical Bulletin》2005,54(4):1046-1047
High (Z)-stereoselectivity of olefination of methyl α-phenylthioalkyl and methyl α-phenylthioalkenyl ketones with methyl trimethylsilylacetate
decreases in the case of ketones containing a higher alkyl-substituent in place of the methyl group.
Dedicated to Corresponding Member of the Russian Academy of Sciences E. P. Serebryakov on the occasion of his 70th birthday.
__________
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 1020–1021, April, 2005. 相似文献
997.
The crystal-chemical structure of the minerals and inorganic compounds kuznetsovite [Hg3](AsO4)Cl and terlinguaite [Hg3][HgO2]Cl2, as well as [Hg3]3(AsO4)4 and [Hg3]2[HgO2](PO2 and their analogs, is considered from the viewpoint of the packing of large supramolecular atomic groups. The cationic layer of polyhedra around the large [Hg3]4+ cations, alternating with the anionic layer of [HgO2]2-, (AsO4)3-, (PO4)3-, Cl-, plays the major role in structure formation. Segregation of mercury cations of different valences possibly reflects the solid-state transformations occurring in nature and accompanied by mercury liberation. 相似文献
998.
Mosstafa Kazemi 《合成通讯》2020,50(13):1899-1935
AbstractCatalysis research under magnetically recoverable nanocatalysts is a well-known topic in organic synthesis. In recent times, catalysis research has clearly experienced a renaissance in the area of utility of ferrite nanoparticles based on their ability to recovery and reusability. In this review, the focus is on the fabrication, characterization and of application the MFe2O4 (M=Co, Cu, and Ni) nanocatalysts in synthesis of heterocyclic structural scaffolds. 相似文献
999.
建立了同时测定水产品中四溴双酚A(TBBPA)和六溴环十二烷(HBCD)的超高效液相色谱-串联质谱方法。样品前处理采用QuEChERS方法,均质生物样品用水分散后加乙腈提取,经C_(18)分散固相萃取净化。采用CORTECS~?C_(18)色谱柱(4.6 mm×100 mm×2.7μm)分离,以甲醇-水为流动相进行梯度洗脱,流速为0.7 mL/min。采用电喷雾离子源,在负离子模式下以多反应监测(MRM)方式检测。结果表明,TBBPA和3种HBCD单体在0.5~500μg/L范围内线性良好,相关系数(r)大于0.998,检出限(LOD,S/N=3)和定量下限(LOQ,S/N=10)分别为0.04~0.16μg/kg和0.12~0.55μg/kg。在5、20、50μg/kg加标水平下的平均回收率为74.0%~121%,相对标准偏差(RSD)为0.20%~23%。该方法操作简单、快速、重现性好,适用于水产品中TBBPA和HBCD的快速检测。 相似文献
1000.