二安替比林（3,4—二甲氧基）苯基甲烷光度法测定茶叶中锰

在碱性介质中，加热时空气氧化Ｍｎ为Ｍｎ，Ｍｎ与二安替比林苯基甲烷反应生成橙色产物，吐温２０和乳酸起到协同增敏作用，λｍａｘ＝４６０ｎｍ，ε＝７．８×１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，锰量在０－１２μｇ／２５ｍｌ范围内符合比尔定律。     

Allyl protecting group mediated intramolecular aglycon delivery (IAD): synthesis of α-glucofuranosides and β-rhamnopyranosides

The use of allyl protecting group mediated intramolecular aglycon delivery (IAD) as a strategy for intramolecular glycosylation has been extended to allow the stereoselective synthesis of α-glucofuranosides and β-rhamnopyranosides, in a totally stereoselective fashion. The efficiency of intramolecular glycosylation is dependent on the protecting group pattern of the glycosyl donor, and on the steric bulk of the glycosyl acceptor.     

铁(Ⅲ)-邻菲罗啉溶液体系的光化学还原 Ⅱ.气相色谱法研究光化反应机理

关于Fe(Ⅲ)-邻菲罗啉(phen)溶液的光化学还原现象的记载可追溯到十九世纪末。     

Fe(110)面上CO化学吸附状态的吸附历史依赖关系

Fe(110)面上直接在室温时吸附的CO同先在170 K吸附然后升温到室温的CO吸附有所不同. 前者有解离而后者无解离; 另外, 前者的饱和吸附量比后者低. 这可以用前者发生了解离来解释. 根据以上结果, 提出了以下的设想, Fe(110)面上的CO解离除了需要足够的热能而外, 还需要在表面的吸附位上有邻近的其它未被覆盖Fe原子的存在, 即需要一定的表面结构.     

NBR/ORGANOMODIFIED BENTONITE INTERCALATED HYBRIDS AND THEIR EFFECTS ON THE TOUGHNESS OF PVC

Hybrids of intercalative nitrile-butadiene rubber/organomodified bentonite (NBR/OMB) were prepared by thelatex intercalation technique. Investigation of their mechanical properties and the microstructore of NBR/OMB showed thatthe organomodified bentonite is an effective toughener for NBR. Transmission electronic microscopy (TEM) and X-rnydiffraction (XRD) tests showed that the NBR macromolecule could be intercalated into the galleries of bentonite.Incorporation of NBR/OMB hybrids as tougheners into poly(vinyl chloride) (PVC) results in a substantial increase in theimpact strength of PVC, but little decrease in its tensile strength and flexural strength, compared to the unmodified PVC.     

Dicopper(I) oxalate complexes as molecular precursors for the deposition of copper compounds

The synthesis, characterization, and thermal decomposition behavior of dicopper(I) oxalato complexes L₄Cu₂(C₂O₄) (L = CNtBu (2a), CNCMe₂CH₂tBu (2b), CNC₆H₃Me₂-2,6 (2c)) is reported. 2c can be prepared in a straightforward manner by the reaction of stoichiometric amounts of Cu₂O and oxalic acid with four equivalents of CNC₆H₃Me₂-2,6, while those complexes with aliphatic isocyanides are better prepared from a copper(I) oxalato complex with alkine capping ligands (Me₃SiCCSiMe₃)₂Cu₂(C₂O₄) (1) via ligand exchange. Crystallographic and spectroscopic evidence for 2a-c confirms the anticipated dinuclear structure with the oxalate in a μ-1,2,3,4 bridging mode and an essentially σ-character of the terminal isocyanides. In solid form the complexes are stable at room temperature and can be handled in air for some time. Their decomposition was studied by thermal gravimetric analysis coupled with mass spectrometry, and the degradation pathway was shown to depend on the type of isocyanide capping ligand. Decomposition of 2a,b takes place between 150 and 200 °C to give CuCN in a clean process that involves isobutene elimination from the terminal ligands, with elimination of (CN)₂ and conversion to elemental copper at higher temperatures. Heating of 2c leads to CuO (and then to Cu₂O) via release of the intact isocyanide, CO₂, and CO in a well-behaved thermal process around 200-280 °C.     

Study on antimony oxide self-assembled inside HZSM-5

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.     

Synthesis of 1,2-bis(methoxyamino)cycloalkanes from alicyclic 1,2-bis(hydroxyamines)

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.     

The first example of the C-3 alkylation of indoles with cyclopropyl ketones promoted by CeCl3·7H2O/LiI

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.     

氮杂冠醚与碱金属离子配位反应的研究

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…