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1.
R. M. Vafina A. T. Gubaidullin O. N. Kataeva I. A. Litvinov Yu. G. Shtyrlin E. N. Klimovitskii 《Russian Journal of Organic Chemistry》2006,42(10):1563-1567
Conformationally heterogeneous 2-substituted 1,3-dithiacyclohept-5-enes (R = Ph, Me, t-Bu), which exist in solution as chair and boat conformers, react with dimethyl 1,2,4,5-tetrazine-3,6-dicarboxylate with high exo-diastereoselectivity: only the chair conformer is involved. The steric structure of 4-methyl-3,5-dithia-9,10-diazabicyclo[5.4.0]undeca-7,10-diene was determined by X-ray analysis. Its crystal packing and supramolecular structure were also analyzed. 相似文献
2.
Summary Optically pure (+)-beta-eudesmol is a possible starting material for the synthesis of several termite defense compounds. A
two step procedure for the isolation of gram quantities of (+)-beta-eudesmol from commercially availableAmyris balsamifera oil (syn. West Indian sandalwood oil), containing 8% beta-eudesmol, was developed. Step one consisted of an efficient vacuum
distillation of the total oil. Step two was a medium pressure LC separation with an AgNO3 impregnated silica gel stationary phase. Several other separation procedures failed due to the presence of many closely related
sesquiterpene alcohols (75% of the oil). 相似文献
3.
V. Yu. Fedorenko R. N. Baryshnikov B. I. Khairutdinov R. M. Vafina Yu. G. Shtyrlin V. V. Klochkov E. N. Klimovitskii 《Russian Journal of Organic Chemistry》2005,41(2):293-297
4-R-3,5-Dioxabicyclo[5.1.0]octanes were prepared in good yields by reduction of the corresponding 8,8-dichloro derivatives in a system Li-t-BuOH. According to the data of dynamic 1H and 13CNMR spectroscopy involving experiments in the NOESY mode the formal (R = H) at −93°C in (CD3)2CO exists in nearly equally occupied chair forms with endo- and exo-oriented three-membered ring. The like structure were found in the diastereomeric 4-Me(t-Bu)-analogs. The characteristic feature of 13C NMR spectra consists in considerable difference in the chemical shifts of the C8 atoms (Δδ∼16–17 ppm). The data on epimerization of diastereomers and calculations along AM1 procedure suggest for formal a three-component equilibrium including a twist-form.__________Translated from Zhurnal Organicheskoi Khimii, Vol. 41, No. 2, 2005, pp. 301–305.Original Russian Text Copyright © 2005 by Fedorenko, Baryshnikov, Khairutdinov, Vafina, Shtyrlin, Klochkov, Klimovitskii. 相似文献
4.
E. N. Klimovitskii V. V. Klochkov M. B. Timirbaev P. P. Chernov A. V. Aganov B. A. Arbuzov 《Russian Chemical Bulletin》1983,32(5):966-969
Conclusions By means of dynamic13C NMR, spectra have been obtained for the frozen chair and twist conformers of phthalylformal and its 2-phenyl derivative. The -effects of the phenyl substituent have been analyzed for both conformational species. 2. The introduction of a phenyl group into position 2 of phthalylformal is not reflected in the magnitude of the conformational free energy.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 5, pp. 1068–1071, May, 1983. 相似文献
5.
Alexander M. Polozov Alexander V. Khotinen Eugene N. Klimovitskii 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4):581-584
Abstract. The X-ray crystal structure of 2-(2′,4′-dioxo-3′-pentyl)-5,5-dimethyl-2-oxo-1,3,2-dioxaphosphorinane (2) reveals significant half-chair distortion of the axially oriented cisenol ring. The molecule also undergoes in-plane deformations. R(O...O) = 2.410 Å in the enol moiety indicates a very strong hydrogen bonding. The enol content, δOH and thermodynamic parameters for the axial-equatorial conformational and keto-enol equilibriums were obtained from 1H, 31P NMR and IR measurements in comparison with the planar 4,6-dimethyl isomer (1) containing equatorially oriented enol ring. The X-ray single crystal structure of 5,5-dimethyl-2-(methoxycarbonyl-3′-oxo-2′-butyl)-2-oxo-1,3,2-dioxaphosphorinane (3) reveals the unusual half-chair conformation of the dioxaphosphorinane cycle disposed a trans-enol ring substituent. 1H, 31P NMR and IR solution data support the same structure displays a strong conformational preference while the minor forms are chair conformers with an axial or equatorial cis-enol ring. 相似文献
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10.
Valeriya A. Startseva Olga A. Lodochnikova Alexander E. Klimovitskii Alexander V. Aref’ev Nadezhda P. Artemova 《Phosphorus, sulfur, and silicon and the related elements》2013,188(5):615-629
Abstract The oxidation of a β-hydroxysulfide in the pinane series by use of m-chloroperbenzoic acid resulted in the formation of the corresponding β-hydroxysulfoxide as a mixture of two diastereomers in 4:5 ratio. According to single-crystal X-ray diffraction (XRD) results, it is established that the diastereomeric mixture of sulfoxides crystallizes in the “racemic compound-like” manner under formation of asymmetric dimers through S=O··H–O interactions. This asymmetric dimer formed from diastereomeric molecules is a structural unit in both crystal modifications, the triclinic and the monoclinic one. The behavior of the diastereomeric mixture of pinane derived sulfoxides in crystals, melts and in tetrachloromethane solutions was studied by IR spectroscopy. The density functional theory (DFT) method with 6-31G (d, p) basis set was used to calculate the optimized geometrical parameters and vibrational frequencies of different associates in solutions. The calculated vibrational frequencies are compared with experimental IR spectra. 相似文献