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非均相催化剂(钯碳催化剂)一般会将芳香酮彻底还原至亚甲基产物,而不易得到苄醇类的中间还原产物.本文报道一系列氨基酮用钯碳催化剂催化氢化的结果,随酮底物含有不同种类的氨基而得到不同的氢化产物(亚甲基产物或二级醇产物),部分则不发生还原反应;分析讨论了底物所含氨基对产物的影响及其机理.结果表明,这是一个制备胺基芳香仲醇的有效方法. 相似文献
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硼氢化钠是一种温和、高选择性的亲核还原剂。一般它只能还原醛、酮和酰氯,而对其它功能团不起作用。因而其应用范围有一定的限制。据文献报道,某些金属卤化物能有效地提高硼氢化钠的还原性能[1]。复合还原剂硼氢化钠/三氯化铁已应用于将β-二烷基氨基共轭烯酮还原为相应的饱和γ-氨基醇[2]。本文研究了硼氢化钠/三氯化铁对亚砜的还原反应。 相似文献
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()呐醇是有机合成中的重要中间体[1],广泛应用于农药、医药等精细化工品的合成;作为能够构建碳碳键的一个重要反应,羰基化合物还原偶联为()呐醇的反应一直是有机合成领域中的一个重要研究课题;同时又形成了两个手性中心,光学活性的邻二醇可作为手性配体广泛应用于手性拆分与不对称合成,特别是在生物活性的天然化合物[2]的合成.1973年,Mukaiyama[3]首次将低价钛运用于醛酮的还原偶联反应,此后随着还原体系的改进和扩充,利用低价钛配合物合成()呐醇的研究也在逐步深入,近年来已有诸多文献报道[4,5]. 相似文献
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Y. Akishige H. Shigematsu T. Tojo H. Kawaji T. Atake 《Journal of Thermal Analysis and Calorimetry》2005,81(3):537-540
Summary Specific heats on the single crystals of Sr2Nb2O7, Sr2Ta2O7 and (Sr1-xBax)2Nb2O7 were measured in a wide temperature range of 2-600 K. Heat anomalies of a λ-type were observed at the incommensurate phase transition of TINC (=495 K) on Sr2Nb2O7 and at the super-lattice phase transition of TSL (=443 K) on Sr2Ta2O7; the transition enthalpies and the transition entropies were estimated. Furthermore, a small heat anomaly was observed at the low temperature ferroelectric phase transition of TLOW (=95 K) on Sr2Nb2O7. The transition temperature TLOW decreases with increasing Ba content x and it vanishes for samples of x>2%. 相似文献
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Kerstin Schulze‐Matthi Jürgen Bendig Petra Neubauer Burkhard Ziemer 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(6):e257-e258
The bonding geometry of sulfur in the cations of the title compounds, C8H11S+·CF3SO3? and C13H13S+·CF3SO3?, respectively, is similar and is independent of the ratio of the Me/Ph substituents. As expected, in both cations, the S—Ph bonds are somewhat shorter than the S—Me bonds. In both crystal structures, the interaction between cations and anions is similar. 相似文献
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Ming‐Liang Tong Shao‐Liang Zheng Xiao‐Ming Chen 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(8):960-962
The title compound, poly[[diaquadibromocadmium‐μ‐(1,3,5,7‐tetraazatricyclo[3.3.1.13,7]decane‐N1:N5)‐aquacadmium‐di‐μ‐bromo‐aquacadmium‐μ‐(1,3,5,7‐tetraazatricyclo[3.3.1.13,7]decane‐N1:N5)‐di‐μ‐bromo] dihydrate], [Cd3Br6(C6H12N4)2(H2O)4]·2H2O, is made up of two‐dimensional neutral rectangular coordination layers. Each rectangular subunit is enclosed by a pair of Cd3(μ2‐Br)6(H2O)3 fragments and a pair of (μ2‐hmt)Cd(H2O)2Br2(μ2‐hmt) fragments as sides (hmt is hexamethylenetetramine). The unique CdII atom in the Cd2Br2 ring in the Cd3(μ2‐Br)6(H2O)3 fragment is in a slightly distorted octahedral CdNOBr4 geometry, surrounded by one hmt ligand [2.433 (5) Å], one aqua ligand [2.273 (4) Å] and four Br atoms [2.6409 (11)–3.0270 (14) Å]. The CdII atom in the (μ2‐hmt)Cd(H2O)2Br2(μ2‐hmt) fragment lies on an inversion center and is in a highly distorted octahedral CdN2O2Br2 geometry, surrounded by two trans‐related N atoms of two hmt ligands [2.479 (5) Å], two trans‐related aqua ligands [2.294 (4) Å] and two trans‐related Br atoms [2.6755 (12) Å]. Adjacent two‐dimensional coordination sheets are connected into a three‐dimensional network by hydrogen bonds involving lattice water molecules, and the aqua, bromo and hmt ligands belonging to different layers. 相似文献
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Summary We have fabricated glasses in the Bi-2223 HTc superconductor system with Bi2Sr2Ca2Cu3-xErxO10+ δ nominal composition, where x=0.5 and 1.0, by the glass-ceramic technique. Using an analysis developed for non-isothermal crystallization studies, information on some aspects of crystallization temperature and thermal properties has been obtained. The crystallization studies were made using DTA with several uniform rates. The calculations of crystallization activation energies, Ea, and the Avrami parameters, n, were made based on the non-isothermal kinetic theory of Kissinger and the Ozawa’s equations. The DTA data of the samples showed that the first crystallization temperature, Tx1, increases and the second crystallization temperature, Tx2, decreases by increasing the Er concentration. This suggests that the Er substitution had significant effect on the glassification of the BSCCO material due to change on the surface nucleation and increased ionic activities at high temperature region. The activation energy for crystallization, Ea, of the samples was also showed an increase at high Er concentration case. However, the Avrami parameter, n, decreased from 2.5 to 1.7 for x=0.5 and 1.0 samples, respectively. This suggests that the growth mechanism is diffusion-controlled and three-dimensional parabolic growth takes place near the first crystallization temperature. The oxidization rates and the activation barrier for oxygen out-diffusion process, E, was calculated using the TG data. It was found that the total mass gain in the x=0.5 sample is comparably smaller than that of the x=1.0 sample. This shows that the oxygen absorption of the x=1.0 sample is faster than the x=0.5 sample, leading to increase in the oxidization rate in the x=1.0 material. 相似文献
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Hiroki Akutsu Jun‐ichi Yamada Shin'ichi Nakatsuji 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(8):o433-o434
The title compound, C24H20P+·C9H17NO5S−, consists of an organic monovalent cation and an organic monovalent anion, the latter being derived from the TEMPO radical (TEMPO is 2,2,6,6‐tetramethylpiperidin‐1‐oxyl). Two inversion‐related anions interact via two –O—H⃛O—S– hydrogen bonds, forming a dimer in which there are no short contacts between the spin centres (–N—O) of the TEMPO(OH)SO3− anions. Furthermore, no significant magnetic interaction is observed between the dimers because the dimer is surrounded by cations. These results are consistent with the paramagnetic behaviour of the title salt. 相似文献
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Maren Pink Doyle Britton Wayland E. Noland Matthew J. Pinnow 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(10):1271-1273
The molecular structures of the title compounds, 2,4,6‐trichlorophenylisonitrile (IUPAC name: 2,4,6‐trichlorophenyl isocyanide), C7H2Cl3N, and 2,4,6‐trichlorobenzonitrile, C7H2Cl3N, are normal. The two structures are not isomorphous, but do contain similar two‐dimensional layers in which pairs of molecules are held together by pairs of Cl?CN [3.245 (3) Å] or Cl?NC [3.153 (2) Å] interactions. The two‐dimensional isomorphism is lost through different layer‐stacking modes. 相似文献
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9,10‐Diphenyl‐9,10‐epidioxyanthracene and 9,10‐dihydro‐10,10‐dimethoxy‐9‐phenylanthracen‐9‐ol
Anwar Usman Hoong‐Kun Fun Yun Li Jian‐Hua Xu 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(6):o308-o310
9,10‐Diphenyl‐9,10‐epidioxyanthracene, C26H18O2, (I), was accidentally used in a photooxygenation reaction that produced 9,10‐dihydro‐10,10‐dimethoxy‐9‐phenylanthracen‐9‐ol, C22H20O3, (II). In both compounds, the phenyl rings are approximately orthogonal to the anthracene moiety. The conformation of the anthracene moiety differs as a result of substitution. Intramolecular C—H⃛O interactions in (I) form two approximately planar S(5) rings in each of the two crystallographically independent molecules. The packing of (I) and (II) consists of molecular dimers stabilized by C—H⃛O interactions and of molecular chains stabilized by O—H⃛O interactions, respectively. 相似文献
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L. Abbas L. Bih A. Nadiri Y. El Amraoui H. Khemakhem D. Mezzane 《Journal of Thermal Analysis and Calorimetry》2007,90(2):453-458
Thermal and chemical durability studies of the phosphate glasses belonging to the binary MoO3-P2O5 and the ternary K2O-MoO3-P2O5 systems are reported. The chemical resistant attack tests carried out on the free alkaline MoO3-P2O5 glasses show that the glass associated with the P/Mo ratio 2 has the high chemical durability. It shows also a high glass
transition temperature value. The above findings are interpreted in terms of the cross-link density of the glasses and the
strength of the M-O bonds (M=P, Mo).
The influence of K2O addition on the properties (density, T
g, durability) of this binary high water resistant glass is studied. It is found that the chemical durability along with the
other physical properties are reduced by the incroporation of K2O in the glass matrix. The results were explained by assuming the formation of non-bridging oxygens and weak bonds. The mechanism
of the dissolution of these glasses is proposed. 相似文献
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Phase equilibria in the LiF-LiCl-LiVO3-Li2SO4-Li2MoO4 system have been studied by differential thermal analysis. The eutectic composition has been determined as follows (mol %): LiF, 17.4; LiCl, 42.0; LiVO3, 17.4; Li2SO4, 11.6; and Li2MoO4, 11.6, with the melting temperature equal to 363°C and the enthalpy of melting equal to (284 ± 7) kJ/kg. 相似文献
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M. G. Zuev 《Russian Journal of Inorganic Chemistry》2007,52(3):424-426
The phase composition has been studied and an equilibrium phase diagram has been designed for the Al2O3-Li2O-R2O5 (R = Ta or Nb) systems in the subsolidus region up to 1000°C and 85 mol % Li2O. New phases with the composition Li1+x Al1?x O2?x , where x = 0–0.67, have been found. 相似文献