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81.
Norma Sbarbati Nudelman Cecilia E. Silvana Alvaro 《Journal of Physical Organic Chemistry》2011,24(11):1067-1071
Inter‐ and intramolecular hydrogen bonding play an important role in determining the arrangement, physical properties, and reactivity of a great diversity of structures in chemical and biological systems. Several aromatic nucleophilic substitutions (ANS) in nonpolar aprotic, (non‐HBD), solvents recently studied in our laboratory have demonstrated the importance of self‐association of amines by hydrogen‐bond interactions. In this paper, we describe 1H‐NMR studies carried out at room temperature on bi‐ and polyfunctionalized amines, namely: N‐(3‐amino‐1‐propyl)morpholine (3‐APMo), histamine, 2‐guanidinobenzimidazole (2‐GB), 1,2‐diaminoethane (EDA), 3‐dimethylamino‐l‐propylamine (DMPA), and 1‐(2‐aminoethyl)piperidine (2‐AEPip). By 1H‐NMR measurements of amine solutions at variable concentrations we have shown that 3‐APMo, histamine and 2‐GB are able to form a six‐membered ring by intramolecular hydrogen bonding, while EDA, DMPA, and 2‐AEPip form dimers by intermolecular hydrogen bonds. Likewise, variable concentration 1H‐NMR studies allowed estimation of the corresponding equilibrium constants for the dimerization. These results are correlated with experimental kinetic results of ANS, confirming hereto the relevance of the “dimer mechanism” in reactions involving these amines. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
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Vignaduzzo SE Maggio RM Castellano PM Kaufman TS 《Analytical and bioanalytical chemistry》2006,386(7-8):2239-2244
Two new analytical methods have been developed as convenient and useful alternatives for simultaneous determination of hydrochlorothiazide
(HCT) and propranolol hydrochloride (PRO) in pharmaceutical formulations. The methods are based on the first derivative of
ratio spectra (DRS) and on partial least squares (PLS) analysis of the ultraviolet absorption spectra of the samples in the
250–350-nm region. The methods were calibrated between 8.7 and 16.0 mg L−1 for HCT and between 14.0 and 51.5 mg L−1 for PRO. An asymmetric full-factorial design and wavelength selection (277–294 nm for HCT and 297–319 for PRO) were used
for the PLS method and signal intensities at 276 and 322 nm were used in the DRS method for HCT and PRO, respectively. Performance
characteristics of the analytical methods were evaluated by use of validation samples and both methods showed to be accurate
and precise, furnishing near quantitative analyte recoveries (100.4 and 99.3% for HCT and PRO by use of PLS) and relative
standard deviations below 2%. For PLS the lower limits of quantification were 0.37 and 0.66 mg L−1 for HCT and PRO, respectively, whereas for DRS they were 1.15 and 3.05 mg L−1 for HCT and PRO, respectively. The methods were used for quantification of HCT and PRO in synthetic mixtures and in two commercial
tablet preparations containing different proportions of the analytes. The results of the drug content assay and the tablet
dissolution test were in statistical agreement (p < 0.05) with those furnished by the official procedures of the USP 29. Preparation of dissolution profiles of the combined
tablet formulations was also performed with the aid of the proposed methods. The methods are easy to apply, use relatively
simple equipment, require minimum sample pre-treatment, enable high sample throughput, and generate less solvent waste than
other procedures.
Electronic supplementary material Supplementary material is available in the online version of this article at and is accessible for authorized users. 相似文献
85.
Hutchison JM Lindsay HA Dormi SS Jones GD Vicic DA McIntosh MC 《Organic letters》2006,8(17):3663-3665
[reaction: see text] The synthesis of an advanced intermediate in the synthesis of the title compound has been achieved. Key steps include an Ireland-Claisen rearrangement to install the C7 tertiary alcohol stereocenter, an SN2' reaction of an alkoxymethyl Cu reagent, and a diastereoselective Re-catalyzed allylic alcohol transposition. 相似文献
86.
The essential oil from aerial parts (stems and leaves) of Atriplex undulata (Moq) D. Dietr. (Chenopodiaceae) has been studied for its in vitro antioxidant activity. The chemical composition of the oil obtained by hydrodistillation was determined by GC and GC-MS. The major constituents were p-acetanisole (28.1%), beta-damascenone (9.3%), beta-ionone (5.1%), viridiflorene (4.7%) and 3-oxo-alpha-ionol (2.2%). The antioxidant activity of the oil was determined by two methods: Crocin bleaching inhibition (Krel = 0.72 +/- 0.15) and scavenging of the DPPH radical (IC50 = 36.2 +/- 1.6 microg/mL). The presence of active compounds like p-acetanisole, carvone, vanillin, 4-vinylguaiacol, guaiacol, terpinen-4-ol and alpha-terpineol could explain the antioxidant activity observed for this oil. 相似文献
87.
We characterize the hereditary torsion pairs of finite type in the functor category of a ring R that are associated to tilting torsion pairs in the category of R-modules. Moreover, we determine a condition under which they give rise to TTF triples. 相似文献
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