纳米晶LaMnO3及La1-xSrxMnO3的合成及其催化氧化性能

纳米晶ＬａＭｎＯ３及Ｌａ１－ｘＳｒｘＭｎＯ３的合成及其催化氧化性能刘源秦永宁（天津大学化工系，天津３０００７２）韩森（天津大学化工系一碳化工国家重点实验室，天津３０００７２）关键词纳米晶，钙钛矿型复合氧化物，一氧化碳，催化氧化，超临界干燥分类号Ｏ６４...     

浆态床FT合成中铁催化剂的穆斯堡尔谱

浆态床ＦＴ合成中铁催化剂的穆斯堡尔谱赵玉龙，李哲（中国科学院山西煤炭化学研究所煤转化国家重点实验室，太原）（中国科学院地质研究所，北京）关键词穆斯堡尔谱，铁催化剂，浆态床ＦＴ合成ＦＴ合成铁系催化剂的穆斯堡尔谱的研究工作已经发表很多，但是浆态操作条件下...     

炭化树脂负载杂多酸催化剂的制备和表征

炭化树脂负载杂多酸催化剂的制备和表征高峰孙经武（天津大学应用化学系，天津３０００７２）钟顺和（天津大学化学工程系，天津３０００７２）关键词炭化树脂，磷钨酸，负载型催化剂，烷基化反应分类号Ｏ６４３杂多酸作为一种新型的多功能催化剂正日益受到人们的关注［...     

甲烷二氧化碳重整制合成气的镍基催化剂性能 Ⅰ.制备条件和载镍量的影响

甲烷二氧化碳重整制合成气的镍基催化剂性能Ⅰ．制备条件和载镍量的影响许峥李玉敏张继炎张鎏（天津大学化工系，天津３０００７２）韩森何菲（天津大学碳一化工国家重点实验室，天津３０００７２）关键词甲烷，二氧化碳，重整，镍，氧化铝，负载型催化剂甲烷二氧化碳重整...     

合成二甲醚铜基/HZSM-5催化剂的研究 制备条件和反应条件对催化剂活性的影响

合成二甲醚铜基／ＨＺＳＭ５催化剂的研究制备条件和反应条件对催化剂活性的影响李增喜冯玉龙王日杰张继炎（天津大学化工系，天津３０００７２）王延吉（河北工业大学化工系，天津３００１３０）韩森（天津大学Ｃ１化工国家重点实验室，天津３０００７２）关键词...     

Nd—Fe—Co—B永磁合金的磁性和穆斯堡尔效应的研究

本文研究了Nd_(17)(Fe_(1-x)Co_x)_(75)B_8(x=0,0.05,0.1,0.2和0.3)永磁合金的磁性和穆斯堡尔谱。得到了合金中四方相、富B相和富Nd相的穆斯堡尔参数——同质异能位移、电四极分裂和超精细场随Co含量的变化关系;根据合金中各含铁物相及四方相中各铁晶位的穆斯堡尔亚谱面积定量估算了各物相的体积分数和铁、钴原子在四方相各晶位的分布情况;由四方相穆斯堡尔谱第2与第3条谱线的强度比计算了合金的磁矩取向角。并从上述穆斯堡尔谱中获得的微观结构方面的结果讨论了合金的剩磁、矫顽力和居里温度。     

中心氧三核过渡金属羰基簇合物的穆斯堡尔谱研究

中心氧三核过渡金属羰基簇合物的穆斯堡尔谱研究王友桐（中国科学院福建物质结构研究所，福州，３５０００２）关键词：三核簇合物，穆斯堡尔谱学引言由于三重桥氧三核铁、铬羰基簇合物具有特殊的结构特征、磁性、催化性能和电子特性，已引起了许多学者的兴趣￣［１－３］...     

铁铈氧化物程序升温还原过程的研究

运用原位穆斯堡尔谱、XRD测定等方法剖析了铁铈氧化物的程序升温还原过程。结果表明，金属离子间的相互作用使得氧化铁的还原温度升高，还原反应活化能提高，抗还原能力增强。     

新型层状混合金属簇合物Fe2Mo2Te4和Fe2Ta2Te4的穆斯堡尔研究

本文测定了新型层状混合金属簇合物（ａ）Ｆｅ２Ｍｏ２Ｔｅ４和（ｂ）Ｆｅ２Ｔａ２Ｔｅ４的穆斯堡尔谱。由穆斯堡尔参数确定这两个簇合物的Ｆｅ原子都属高自旋＋３价，处四面体配位中心。簇合物（ａ）中两个铁原子是等价的，而簇合物（ｂ）中两铁原子却是不等价的，这是由于簇合物（ｂ）中Ｆｅ１原子的构型畸变比Ｆｅ１原子大的缘故。     

铁/活性炭催化剂的氮化及其碳化行为

用原位穆斯堡尔谱考察了不同担载量的Ｆｅ／ＡＣ催化剂的氮化以及随后的碳化行为。Ｆｅ／ＡＣ催化剂经５００℃Ｈ预还原后，于３５０℃流动态氨气中氮化５小时可生成ε－氮化铁，其穆斯堡尔谱呈双峰（δ～０．４２ｍｍ／ｓ，△～０．３２ｍｍ／ｓ）。再在合成气（２Ｈ２／ＣＯ）中进行碳化处理，ε－氮化铁中的氮原子可逐渐被碳原子取代而转化为氮碳化铁和碳化铁，但铁的担载量越高，这种取代越困难。８％Ｆｅ／ＡＣ催化剂在２５０℃     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

A carbanion induced synthesis of highly congested pyrazole and imidazole containing heterocycles

An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.