4—CH3SC6H4NH2对α—磷酸锆的插层特性

制备了４－ＣＨ３ＳＣ６Ｈ４ＮＨ２（ＭＭＡ）插层的α－Ｚｒ９ＨＰＯ４）２．Ｈ２Ｏ，研究了不同实验条件下ＭＭＡ的插层特性，发现插层反应与ＭＭＡ和α－ＺｒＰ摩尔比Ｒ有关；（１）当Ｒ〉２时，有插层产物相产生，但是即使在ＭＭＡ大大过量的条件下，仍然有部分α－ＺｒＰ颗粒大小等有关；插层产物的层间距约为２．３６ｎｍ，，层间距的大小不随反应物浓度，温度等条件变化。     

SO^2—4／ZrO2超强酸制备方法的改进

用ＢＥＴ、ＸＲＤ、流动指法剂法、化学分析、低温正丁烷异构化反应等手段研究了制备条件对ＺｒＯ２前驱体和ＳＯ＾２－４／ＺｒＯ２超强酸性能的影响。实验结果表明，采用不同的制备条件，ＺｒＯ２前驱体的比表面可相差１．８倍，ＳＯ＾２－４／ＺｒＯ２的酸强度相差约１０００倍，ＳＯ＾２－４／ＺｒＯ２的正丁烷异构化反应活性相差约３００倍，ＺｒＯ２最高比表面可达２４５ｍ＾２／ｇ，ＳＯ＾２－４／ＺｒＯ２酸强度为Ｈ０≤－１     

THE SYNTHESIS AND CRYSTAL STRUCTURE COMPLEX OF SCHIFF BASE CONTAINING S·N－Cd_3｜CH_3O（O）C_6H_3CH＝NNHC（S）NH_2｜4·（CH_3COO_2·1／2［CH_3S（O）CH_3］·2H_2O

ＴＨＥＳＹＮＴＨＥＳＩＳＡＮＤＣＲＹＳＴＡＬＳＴＲＵＣＴＵＲＥＣＯＭＰＬＥＸＯＦＳＣＨＩＦＦＢＡＳＥＣＯＮＴＡＩＮＩＮＧＳ·Ｎ－Ｃｄ_３｜ＣＨ_３Ｏ（Ｏ）Ｃ_６Ｈ_３ＣＨ＝ＮＮＨＣ（Ｓ）ＮＨ_２｜４·（ＣＨ_３ＣＯＯ_２·１／２［ＣＨ_３Ｓ（Ｏ）ＣＨ_３］·?..     

α-磷酸锆层柱材料的制备、表征及其催化羰基化性能

采用配体４－ＣＨ３ＳＣ６Ｈ４ＮＨ２插层的α－磷酸锆为插层主体,将Ｒｈ６３＋引入层状材料的层析之间制备了新型层柱催化材料Ｚｒ（ＨＰＯ４）１．７０（ＣＨ３ＳＣ６Ｈ４ＮＨ２）１．０９（ＰＯ４）０．３０Ｒｈ０．１０．５．５２Ｈ２Ｏ,其是距为２．３６变为１．５６ｎｍ,结晶度有所下降。     

SO_4~（2－）／ZrO_2超强酸制备方法的改进

用ＢＥＴ、ＸＲＤ、流动指示剂法、化学分析、低温正丁烷异构化反应等手段研究了制备条件对ＺｒＯ２前驱体和ＳＯ／ＺｒＯ２超强酸性能的影响．实验结果表明，采用不同的制备条件，ＺｒＯ２前驱体的比表面可相差１．８倍，ＳＯ／ＺｒＯ２的酸强度相差约１０００倍．ＳＯ／ＺｒＯ２的正丁烷异构化反应活性相差约３００倍．ＺｒＯ２最高比表面可达２４５ｍ２／ｇ，ＳＯ／ＺｒＯ２酸强度为Ｈ０≤－１．６０，２０℃时ＳＯ／ＺｒＯ２正丁烷异构化反应速率常数为１５．５×１０－３ｈ－１。     

THE SYNTHESIS AND STRUCTURE OF A NEW MICROPOROUS BERYLLOPHOSPHATE （BeHPO＿4·H＿2O）

ＴＨＥ　ＳＹＮＴＨＥＳＩＳ　ＡＮＤ　ＳＴＲＵＣＴＵＲＥ　ＯＦ　Ａ　ＮＥＷ　ＭＩＣＲＯＰＯＲＯＵＳ　ＢＥＲＹＬＬＯＰＨＯＳＰＨＡＴＥ　（ＢｅＨＰＯ＿４·Ｈ＿２Ｏ）￥ＬｏｎｇＹＵ（ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍｉｓｔｒｙ，ＬｉａｏｎｉｎｇＵｎｉｖｅｒｓ...     

Synthesis,Crystal Structure and Studies on the Noncovalent Interaction of [Zn(BpheO)_2(phen)]_2·2CH_3OH·3H_2O

Ｓｙｎｔｈｅｓｉｓ，ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅａｎｄＳｔｕｄｉｅｓｏｎｔｈｅＮｏｎｃｏｖａｌｅｎｔＩｎｔｅｒａｃｔｉｏｎｏｆ［Ｚｎ（ＢｐｈｅＯ）２（ｐｈｅｎ）］２·２ＣＨ３ＯＨ·３Ｈ２ＯＳＨＥＮＬｉａｎｇ＊ａｎｄＳＨＥＮＧＧｕｏ－ｄｉｎｇ（Ｄｅ...     

EPR Study of a New Crystal of the Binuclear Copper（Ⅱ） Cluster Compound－〔Cu_2（α－C_（10）H_7CH_2CO_2）_4－（DMF）_2〕·（DMF）_2·H_2O

ＥＰＲＳｔｕｄｙｏｆａＮｅｗＣｒｙｓｔａｌｏｆｔｈｅＢｉｎｕｃｌｅａｒＣｏｐｐｅｒ（Ⅱ）ＣｌｕｓｔｅｒＣｏｍｐｏｕｎｄ－〔Ｃｕ_２（α－Ｃ_（１０）Ｈ_７ＣＨ_２ＣＯ_２）_４－（ＤＭＦ）_２〕·（ＤＭＦ）_２·Ｈ_２Ｏ￥ＳｕｎＱｉｏｎｇ－Ｌｉ；ＨｕａｎｇＸ?..     

SYNTHESIS OF 4－（2，3－DIMETHOXY－4－ISOPROPYLBENZYL）－3－ETHOXYCARBONYLMETHYL－2－CYCLOHEXENONE

ＳＹＮＴＨＥＳＩＳ　ＯＦ　４－（２，３－ＤＩＭＥＴＨＯＸＹ－４－ＩＳＯＰＲＯＰＹＬＢＥＮＺＹＬ）－３－ＥＴＨＯＸＹＣＡＲＢＯＮＹＬＭＥＴＨＹＬ－２－ＣＹＣＬＯＨＥＸＥＮＯＮＥＳＹＮＴＨＥＳＩＳＯＦ４－（２，３－ＤＩＭＥＴＨＯＸＹ－４－ＩＳＯＰＲＯＰＹ...     

SO^2—4／TiO2和SO^2—4／Fe2O3固体超强酸研究

用ＸＲＤ、ＴＧ－ＤＴＧ、ＳＥＭ和化学分析等手段研究了浸渍Ｈ２ＳＯ４的无定形ＴｉＯ２和Ｆｅ２Ｏ３在焙烧过程中的晶化、相变、失水及失硫情况，总结出ＳＯ＾２－４／ＭｘＯｙ型固体超强酸具有与ＳＯ＾２－４／ＺｒＯ２体系相同的形成规律。用ＩＲ光谱和常温正戊烷异构化反应对ＳＯ＾２－４／ＴｉＯ２／Ｆｅ２Ｏ３的超强酸性进行了表征，表明它们与ＳＯ＾２－４／ＺｒＯ２体系具有相似的表面酸位结构，无水状态主要为Ｌ酸位，吸水     

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.     

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.     

Copper-catalyzed multicomponent reactions of 2-iodoanilines,benzylamines, and elemental sulfur toward 2-arylbenzothiazoles

A relatively cheap copper salt-catalyzed, three-component approach providing 2-arylbenzothiazoles in good to excellent yields from readily available 2-iodoanilines, benzylamines, and sulfur powder is reported. This methodology allows preparation of various classes of 2-arylbenzothiazoles and provides a general, reliable approach.