新的苯并二氮卓类三环化合物：1H，10H4，9－二氢－环戊并［1，2－b］［1，5］苯并二氮卓－10－酮及其3－甲基衍生物的合成

通过邻苯二胺与环戊酮的β－羧酸酯缩合及催化氢化，合成了由环戊基与苯并二氮并环形成的新的苯并二氮类三环化合物。     

芳基肟胺菊酯类化合物和1，2，4－噁二唑衍生物的合成及其生物活性研究

芳基肟胺化合物与取代环丙烷羧酸酰氯在Ｅｔ_３Ｎ作用下室温反应得到芳基肟胺菊酯类化合物，在甲苯中回流反应则得到含取代环丙烷基的１，２，４－　二唑衍生物。前者在甲苯中回流，ＨＯＡｃ作催化剂时发生环化反应也生成１，２，４－　二唑衍生物．初步生物活性测试表明这些化合物具有的杀菌和除草活性．     

N－吡唑啉酮基－α－氨基膦酸酯的合成及其生物活性的研究

Ｎ－吡唑啉酮基－α－氨基膦酸酯的合成及其生物活性的研究龙韫先，张克胜，邱德文（南开大学元素有机化学研究所，天津，３０００７１）关键词氨基膦酸酯，合成，抗病毒活性植物病毒病素有“植物癌症”之称，每年因此造成经济损失多达上百亿美元。因此，国内外的科研工作...     

1，2，4－三嗪类化合物研究（XXIV）──吡唑并－（5，4－e）－1，2，4－三嗪衍生物的合成

先合成１，２，４－三嗪环，然后并接吡唑环，对标题化合物进行了合成研究。对１，２，４－三嗪环上的硫化反应进行了改进，解决了３个反应活性相近部位的选择性肼解问题；并发现了肼基与乙酸乙酯于室温下反应生成１，３，４－　二唑环的新反应。     

手性铜催化剂的制备及在环丙烷羧酯酯不对称合成中的应用

３类手性配体ｄ－１０－樟脑磺酸及其衍生物，α－（－）－羟蒎酮及其衍生物，又恶唑啉６衍生物分别与铜（Ⅱ）形成手性铜配合物，催化重氮乙酸酯与１，１－二苯乙烯或异丁烯的环丙烷化加成反应，得到光学活性环丙羧酸酯，不对称诱导最高可达９５％ｅ．ｅ．。     

二氯菊酸类杀虫剂光学纯度分析方法的研究

报道了旋光性的顺式－2，2－二甲基－3－（2，2－二氯乙烯基）环丙烷羧酸（谷称顺式二氯菊酸）类杀虫剂光学纯度的色谱分析方法。光学活性杀虫剂的顺式－2，2－二甲基－3－（2，2－二氯乙烯基）环丙烷羧酸先与氯化亚砜生成酰氯，一财与S（－）－a-甲基苄胺作用，生成顺式－2，2－二氯－3－异丁烯基环丙烷羧酸非对映异构体的酰胺，经薄层色谱纯，用高效液相色谱进行分析，即可确定中间体的光学纯度。光学纯度一定的中间体经合成至最终产物，其光学纯度保持不变。     

环丙烷甲酸－2－甲基－1－乙炔基－2－戊烯酯的合成

环丙烷甲酸－２－甲基－１－乙炔基－２－戊烯酯的合成涂君 ，于翔，肖蓉（中国科学院成都有机化学研究所，成都６１００４１）日本开发的炔戊菊酯￣［１］、氯戊炔菊酯等￣［２］其蒸气压皆比常用的丙烯菊酯、苯醚菊酯、胺菊酯、苄呋菊酯及炔呋菊酯高数十倍到数百倍。由?..     

二氯菊酯光学异构体的分析

利用顺式二氯菊酯和反式二氯菊酸的溶解度不同及pKa值的差异，分离二氯菊酸中的顺式体和反式体，可取得较好的效果（反式二氯菊酸收率83．7％，顺式二氯菊酸收率88．9％），以S（－）－α－甲基苄胺为拆分剂，对顺式－2，2－二甲基－3－3（2，2－二氯乙烯基）环丙烷羧酸酯（俗称顺式二氯菊酯）类杀虫剂合成中间体0顺式－2，2－二甲基－3－（2，2－二氯乙烯基）环丙烷羧酸（俗称顺式二氯菊酸）进行拆分，可以得到其旋光异构体；其旋光异构体与S（－）－α－甲基苄胺衍生化，生成相应的酰胺；经TLC纯化后，以外消旋顺式二氯菊酸酰胺作为对照，用HPLC检测其旋光异构体的光学纯度；结果显示，顺式－R（＋）－2，2－二甲基－3－（2，2－二氯乙烯基）环丙烷羟酸光学纯度为93．7％，顺式－S（－）－2，2－二甲基－3－（2，2－二氯乙烯基）环丙烷羧酸光学纯度为81．8％，对反式二氯菊酸的光学纯度分析，可采用类似的方法：经顺，反分离，旋光异构体拆分获得的高效中间体，再进行后序合成，其顺反比，旋光纯度不变。     

γ－芳基取代烯丙醇菊酯的合成及杀虫活性

γ－芳基取代烯丙醇菊酯的合成及杀虫活性陈亚娟，黄润秋，马军安（南开大学元素有机化学研究所，天津，３０００７１）关键词γ－芳基取代烯丙醇，拟除虫菊酯，杀虫活性第一个人工合成除虫菊酯烯丙菊酯保留了天然除虫菊酯醇部分的环戊烯醇酮结构，至今仍广泛用作卫生杀虫...     

新磺酰脲类化合物的合成、结构及构效关系研究（Ⅲ）──N－［2＇－（4，6－二甲基）嘧啶基］－2－甲酸乙酯－苯磺酰脲的晶体及分子结构

新磺酰脲类化合物的合成、结构及构效关系研究（Ⅲ）──Ｎ－［２＇－（４，６－二甲基）嘧啶基］－２－甲酸乙酯－苯磺酰脲的晶体及分子结构李正名，贾国锋，王玲秀，赖城明（南开大学元素有机化学国家重点实验室，南开大学元素有机化学研究所，天津，３０００７１）（南...     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

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.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.     

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.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

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.