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991.
Sb/ZSM-5 was obtained by solid-state reaction with the mixture of Sb2O3 and zeolite HZSM-5 under a dry nitrogen flow at 773 K. Characterization of the treated zeolite was undertaken with XRD, 27Al MAS NMR, BET, TGA and FT-IR. The results revealed that part of the antimony oxides migrated into the channels of zeolite, and decreased the Brönsted acid sites in Sb/ZSM-5 remarkably. The other part of antimony oxides together with the amorphous alumino-silicate in the products distributed on the external surface of zeolite ZSM-5 and modified it, while the framework of ZSM-5 in crystal phase was retained. The structure of occluded antimony oxide inside the channels of ZSM-5 was studied by XRD Rietveld method. The result showed that their structure can be described as a chain of non-perfect [Sb5O5(H2O)2]n5n+, which is parallel to the straight channel of ZSM-5. There is about 0.6 [Sb5O5(H2O)2]5+ unit in every cell of the ZSM-5 on an average. 相似文献
992.
D. G. Mazhakin V. K. Khlestkin A. Ya. Tikhonov L. B. Volodarsky 《Russian Chemical Bulletin》1996,45(4):880-884
Derivatives of 1,4-dihydroxypiperazine-2,3-dione were obtained by reaction of cis-1,2-bis(hydroxyamino)cycloalkanes with diethyl oxalate. Their alkylation with CH2N2 or Mel afforded 1,4-dimethoxypiperazine-2,3-diones. Hydrolysis of the latter gave 1,2-bis(methoxyamino)cycloalkanes.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 925–929, April, 1996. 相似文献
993.
Indoles undergo smooth alkylation with cyclopropyl ketones in the presence of the CeCl3·7H2O/LiI reagent system in refluxing acetonitrile under neutral conditions to produce the corresponding C-3 substituted indole derivatives in good to high yields and with high selectivity. The use of CeCl3·7H2O/LiI makes this method simple, convenient, and cost-effective. 相似文献
994.
滴定量效法是研究反应热化学和热力学的重要手段之一.用这种方法对冠醚与金属离子的配位反应热力学性质进行研究一直受到很大关注【且S习.但是对氨杂冠林,尤其是一系列结构相似的氨杂冠醚体系进行系统的热力学性质研究的报导不多.前文K则曾报导了用自组装的消定量热计对银(I)-a吹体系和铜(11)·N,N’一问位取代革基乙二胺体系的配位反应热化学研究结果·本文报导从(对位取代革基)k杂15冠5卜RPW15CS,R=CIZH;CHa;CHso)与碘化钠和碘化钾在25T、无水乙过溶液中进行配位反应的消定量效研究结果.讨论了配体上取代基的电… 相似文献
995.
几种改进的CoMFA方法比较研究血小板活化因子拮抗剂 总被引:6,自引:1,他引:6
由于传统的比较分子场分析(CoMFA)方法本身存在一些缺陷,使得分子的叠合 规则以及叠合分子的空间取向和空间位置等因素对q~2的影响很大,因此相继提出 了几种改进的CoMFA方法。为了优化CoMFA结果,应用传统的CoMFA方法和交叉验证 的R~2引导的区域选择法(q~2-GRS)、全取向搜索法(AOS)、全空间搜索法(APS) 以及比较分子相似性指数(CoMSIA)等四种改进的CoMFA方法,对18个pinusolide类 衍生物这类新发现的血小板活化因子(PAF)拮抗剂进行了比较研究。结果表明四 种改进的CoMFA方法得到的q~2值均比传统CoMFA的高。q~2-GRS方法得到的q~2值有 所提高,但综合结果并不理想,AOS与APS得到的q~2较为理想,而在CoMSIA中, q~2几乎不受空间取向或空间位置的影响。同时我们引人基于样本的偏最小二乘法 (SAMPLS)取代原AOS/APS程序中的传统PLS进行统计分析,明显提高了其运行速 度。最后,根据q~2最高的CoMFA模型和CoMSIA模型设计了几个预测活性更高的 pinusolide类似物。 相似文献
996.
Hans-Georg Henning Giedrius Mazunaitis 《Monatshefte für Chemie / Chemical Monthly》1992,123(1-2):93-98
Summary Irradiation of solutions of excess cyclohexene and 2-acetyl-5,5-dimethyl-1,3-cyclohexanedione (1), and 3-acetyl-1,5,5-trimethyl-2,4-pyrrolidinedione (4) results mainly in the formation of 1,5-diones2 and5. These originate from intermediate cycloadducts of cyclohexene and theexo-enols of the cyclic 1,3-diketones. The yields decrease with increasing polarity of the solvent. In solution2 and5 are in equilibrium with the cyclic hemiacetales3 and6. 相似文献
997.
Borohydride exchange resin-transition metal(Co,Ni,Cu,)compoundsystems reduced C=C double to C-C single bond in ethanol. 相似文献
998.
Shkumbatiuk R Bazel YR Andruch V Török M 《Analytical and bioanalytical chemistry》2005,382(6):1431-1437
A new, simple, rapid, and sensitive spectrophotometric method has been developed for the determination of nitrophenols [picric acid (PA); dinitrophenols (DNP)] in wastewater samples. The method is based on the reaction of nitrophenols with 2-[(E)-2-(4-diethylaminophenyl)-1-ethenyl]-1,3,3-trimethyl-3 H-indolium chloride reagent to form the colored ion associates, which are extracted by organic solvents. The molar absorptivity of the ion associates of PA with the investigated reagent ranges from 8.3×104 to 11.3×104 L mol–1 cm–1, depending on the extractant. Because only PA is extracted in an acidic medium with the investigated reagent, but both PA and DNP are extracted in an alkaline medium, it is possible to determine both substances in a mixture. Appropriate reaction conditions have been established. The absorbance of the colored extracts obeys Beers law in the range of 0.04–4.58 mg L–1 PA, 1.0–18.4 mg L–1 2,4-DNP and 1.2–14.7 mg L–1 2,6-DNP, respectively. The limit of detections, calculated from a blank test (n=10; P=0.95), are 0.05 mg L–1 PA, 0.9 mg L–1 (2,4-DNP), and 1.1 mg L–1 (2,6-DNP), respectively. 相似文献
999.
Luciani G. Costantini A. Branda F. Scardi P. Lanotte L. 《Journal of Thermal Analysis and Calorimetry》2003,72(1):105-111
A traditional TG apparatus was modified by placing two permanent magnets producing a controlled magnetic field (TG(M): Magneto
Thermogravimetry). This technique proved to be useful to study both structural relaxation and crystallisation of ferromagnetic
metallic glasses. Results obtained for the amorphous alloys Fe40Ni40P14B6 and Fe62.5Co6Ni7.5Zr6Nb2Cu1B15, are reported in this paper. Structural relaxation can be evaluated by measuring changes in Curie temperature induced by
thermal treatments. Crystallisation in TG(M) is detected through a change in the measured apparent mass (difference between
the sample mass and magnetic force driving it upward). These results were confirmed by DSC analysis. Whether the obtained
crystalline phase is ferromagnetic, it can be identified through its Curie temperature, measured by TG(M). In fact the value
of 770°C measured as Curie temperature of crystallised Fe62.5Co6Ni7.5Zr6Nb2Cu1B15led to conclude that the only ferromagnetic crystalline phase is a-Fe. These hypothesis was confirmed by XRD analysis, showing
that the first crystallisation yields to a-Fe nanocrystals.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
1000.