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211.
Concha-Graña E Turnes-Carou MI Muniategui-Lorenzo S López-Mahía P Fernández-Fernández E Prada-Rodríguez D 《Journal of chromatography. A》2004,1047(1):147-155
The scope of this work is the development of a rapid, reliable and sensitive method for the analysis of organochlorine pesticides from soils by pressurized liquid extraction (PLE). The effect of four parameters (temperature, pressure, static time and cell volume) on the extraction efficiency was studied. The great extracting power of the PLE causes the extraction of numerous interfering substances, so a more efficient purification of this extract was necessary. In this work several sorbents have also been assayed to carry out the purification of soil samples: Florisil, silica, alumina, carbon, as well as combinations of them. Finally, the proposed analytical method was validated using a certified reference soil material (CRM804-050) and the results were compared with those obtained by other extraction techniques (Soxhlet and microwave-assisted extraction). 相似文献
212.
Tetramethyldisilane-1,2-diyl bridged Dicyclopentadienyl and Diindenyl Metal Dichlorides of the Group 4 Metals – Crystal Structure of Dicyclopentadienyl and diindenyl metal dichlorides of the type Cp′? SiMe2SiMe2? Cp′MCl2 (Cp′ = C5H4, M = Ti ( 1 ), Zr ( 2 ), Hf ( 3 ); Cp′ = C9H7, M = Zr ( 4 ), Hf ( 5 )) were synthesized and characterized by means of their 1H, 13C, 29Si-n.m.r., MS, and IR spectra. The crystal structure of 2 was determined. 相似文献
213.
Proton-active substances react with certain electron-rich olefins with cleavage of the central C?C double bond to give compounds that can be formally regarded as insertion products of nucleophilic carbenes. If they satisfy certain structural conditions, they isomerize with β elimination to give open-chain compounds. Both CH-acidic compounds and compounds containing NH or OH groups can undergo this reaction. The mechanisms are discussed, and the importance of the intermediate products to biochemistry (thiamine, tetrahydrofolic acid) is indicated. 相似文献
214.
215.
Julia E. Barker 《Tetrahedron letters》2005,46(40):6805-6808
Mononuclear (Me3TACN)MnX3 compounds, where X is Cl−, Br−, or N3−, and Me3TACN is 1,4,7-N,N′,N″-trimethyl-1,4,7-triazacyclononane, have been tested for catalyzing both sulfide oxygenation and styrene epoxidation by tert-butyl hydroperoxide (TBHP) and display turnover frequencies (TOF) up to 200 h−1 at room temperature. Sulfoxides or sulfones may be produced selectively by varying reaction conditions. Product distribution from the oxygenation reactions of ethyl phenyl sulfide, 2-chloroethyl phenyl sulfide, and styrene is consistent with a mechanism involving an early single-electron transfer (SET) step. 相似文献
216.
[RhH(CO)(PPh3)2] (1) reacts with Et3N·3HF to give the fluoro compound [RhF(CO)(PPh3)2] (2). In a comparable reaction [RhF(PEt3)3] (5) has been obtained from [RhH(PEt3)3] (3) or [RhH(PEt3)4] (4) with substoichiometric amounts of Et3N·3HF in THF. If the latter reaction is carried out in benzene, the complexes 5, cis-mer-[Rh(H)2F(PEt3)3] (6) and cis-fac-[Rh(H)2F(PEt3)3] (7) are obtained. Treatment of 5 with HCl in ether effects the generation of [RhCl(PEt3)3] (8) and the bifluoride compound [Rh(FHF)(PEt3)3] (9), which can be converted into 5 in the presence of Et3N and Cs2CO3. Treatment of 5 with HSiR2Ph (R=Ph, Me) leads to the formation of 3 and the rhodium(III) silyl complexes fac-[Rh(H)2(SiR2Ph)(PEt3)3] (10: R=Ph, 11: R=Me). 相似文献
217.
Naoki KakusawaYoshinori Tobiyasu Shuji YasuikeKentaro Yamaguchi Hiroko SekiJyoji Kurita 《Tetrahedron letters》2003,44(47):8589-8592
The reaction of 12-arylethynyl-6-methyl-5,6,7,12-tetrahydrodibenzo[c,f][1,5]-azastibocines with organic halides such as acyl halides and aryl halides in the presence of PdCl2(PPh3)2 as a catalyst led to the formation of cross-coupling products, alkynyl ketones and diaryl acetylenes, in good yields. The reactivity of the ethynyl group on the 1,5-azastibocines was far superior to that on diphenyl(phenylethynyl)stibane, which brought about marked improvement in the reaction conditions (lower temperature and shorter reaction time) and in the yields of the cross-coupling products. Single-crystal X-ray analysis of the ethynyl-1,5-azastibocine showed the presence of intramolecular Sb?N interaction which should be responsible for the remarkable reactivity enhancement of the 1,5-azastibocines for this type of reaction. 相似文献
218.
Dawson结构钼钒磷杂多化合物对苯酚过氧化氢羟化作用的研究 总被引:14,自引:0,他引:14
Dawson结构钼钒磷杂多化合物对苯酚过氧化氢羟化作用的研究于剑锋,杨宇,吴通好,孙家锺(吉林大学化学系理论化学研究所,长春,130023)关键词Dawson结构钼钒磷杂多化合物,苯酚羟化,过氧化氢苯二酚(DBH)是重要的化工原料.由芳香化合物羟化制... 相似文献
219.
220.
Condensation of 3,5-dinitro-4-chloro-6-methoxy-2-methylquinoline (1) with benzylamine, ethanolamine and/or thioglycolic acid afforded the quinoline derivatives4 a-c. Cyclization of4 a and4 b with alkali and condensation of1 with glycine in sodium carbonate solution furnish 2H-imidazo[4,5-c]quinoline derivatives5 a-c, respectively. Treatment of5 b with benzaldehyde in presence of zinc chloride gave the styryl derivative6. 1 reacted with sodium azide to give the azido derivative4 d, which upon treatment with phenylhydrazine or sodium borohydride yielded the 4-amino derivative4 3. Moreover,1 was treated with phenylhydrazine to give4 f, which cyclized in 10% sodium hydroxide solution to the corresponding v-triazolo[4,5-c]quinoline 3-oxide derivative7. When however4 f was treated with dilute hydrochloric acid, the corresponding phenylpyrazolo[3,4,5-de]quinoline derivative8 was obtained.
Baseninduzierte Cyclisierung einiger Chinoline. Darstellung höherer Stickstoff-Heterocyclen
Zusammenfassung Kondensation von 3,5-Dinitro-4-chlor-6-methoxy-2-methylchinolin (1) mit Benzylamin, Ethanolamin und/oder Thioglycolsäure ergab die Chinolinderivate4 a-c. Cyclisierung von4 a und4 b mit Alkali und Kondensation von1 mit Glycin in Natriumcarbonatlösung lieferte 2H-imidazo[4,5-c]chinolin-Derivate5 a-c. Behandlung von5 b mit Benzaldehyd in Gegenwart von Zinkchlorid ergab das Styrylderivat6. 1 wurde mit Natriumazid zum Azidoderivat4 d umgesetzt, das mit Phenylhydrazin oder Natriumborhydrid zum 4-Aminoderivat4 e weiterreagierte.1 ergab mit Phenylhydrazin4 f, das in 10% NaOH-Lösung zum entsprechenden Triazolo[4,5-c]chinolin-Derivat7 cyclisierte. Aus4 f wurde mit verdünnter Salzsäure das Phenylpyrazolo[3,4,5-de]chinolin8 erhalten.相似文献