不对称环磷化合物的合成及立体化学（I）：—环磷酰氯和3…

研究了２－氧代－２－氯－４－取代苯基－５，５－二甲基－１，３，２－二氧磷杂环己烷与３－羟基异恶唑的反应，得到的氧磷酰化产物含有顺反两种异构体，用＾１Ｈ ＮＭＲ，＾３１Ｐ ＮＭＲ，Ｘ射线衍射确定了它们的构型，并讨论了亲核取代反应中手性磷原子构型保持和翻转的机理，测定了异构体的生物活性。     

4个新型有机磷缩合试剂的合成及其在生物活性肽合成中…

报道了４个新型有机磷化合物：Ｎ－二乙氧基磷酰并恶唑酮（ＤＥＰＢＯ０，Ｎ－（２－氧－１，３，２－二氧杂磷环己烷基）－苯并恶唑酮（ＤＯＰＢＯ），３－（２′－氧－１′，３′，２′－二氧杂磷杂环己烷基）－氧－１，２，３－苯并三嗪－４（３Ｈ）－酮（）ＤＯＰＢＴ）和３－（二乙氧基磷酰基）－氧－１，２，３－苯并三嗪－４（３Ｈ）－酮（ＤＥＰＢＴ）的合成，并研究了它们作为缩合试剂的多肽合成中的应用，研究结果表明，它     

磷杂螺环化合物的合成——3,9—二氢—3,9—二硫代—2,4,8,10—…

本文合成了３，９－二氢－３，９－二硫代－２，４，８，１０－四氧杂－３，９－二磷杂螺环－［５，５）十一烷２，研究了２在Ｎ，Ｎ－二甲基乙酰胺介质中，在氢化钠作用下与α－芳基－β－硝基烯的加成反应，得到５个新的加成产物３ａ－ｅ，对２及加成物３ａ－ｅ的＾１ＨＮＭＲ谱进行了归属，并得到元素分析和ＩＲ的证实。     

磷杂螺环化合物的合成──3，9－二氢－3，9－二硫代－2，4，8，10－四氧杂－3，9－二磷杂螺环［5，5］十一烷的合成及其与α－芳基－β－硝基烯的加成反应

本文合成了３，９－二氢－３，９－二硫代－２，４，８，１０－四氧杂－３，９－二磷杂螺环－［５，５］十一烷２，研究了２在Ｎ，Ｎ－二甲基乙酰胺介质中，在氢化钠作用下与α－芳基－β－硝基烯的加成反应，得到５个新的加成产物３_（ａ－ｅ），对２及加成物３_（ａ－ｅ）的~１ＨＮＭＲ谱进行了归属，并得到元素分析和ＩＲ的证实。     

含磷稠杂环的合成及其生物活性

研究了氯代膦酰异氰酸酯与５－氨基－３－苄硫基－１，２，４－三唑及其类似物的成环反应，合成了１２个，７－芳基（烷氧基）－２－苄硫基－５，７－二氧代－４，５，６，７－四氢－７－磷杂－１，２，４－三唑（１，５ａ）三嗪，利用ＨＮＭＲ，ＰＮＭＲ确定其为Ｚ型，生物活性测定结果表明，部分化合物具有一定的除草活性。     

不对称1,3,2—二氧磷杂环己烷非对映选择性合成及其生物活性

不对称１，３，２－二氧磷杂环己烷非对映选择性合成及其生物活性邵瑞链＊杨敏华成俊然（南开大学元素有机化学研究所，元素有机化学国家重点实验室天津３０００７１）关键词二氧磷杂环，立体有择合成，顺反异构体，生物活性１９９７－０６－０４收稿，１９９７－１２－０...     

DL－丙交酯与2－氢－2－氧－1，3，2－二氧磷杂环己烷的开环共聚合研究

在三异丁基铝催化下ＤＬ－丙交酯与２－氢－２－氧－１，３，２－二氧磷杂环己烷开环共聚，制备了一类新型水溶性共聚物Ｐ（ＬＡ－ｃｏ－ＴＭＰ）。用１ＨＮＭＲ、ＩＲ谱对其结构进行了表征，并研究了催化剂用量及不同单体配比对总转化率、共聚物组成及特性粘度的影响。     

不对称1,3,2—苯并二氧碳杂环己烷非对映消旋体的合成及生 …

通过相转移催化关环反应合成了新的６－取代－２－硫－２－烷（芳）氧－４（２，４－二氯苯基）－４－氢－１，３，２－苯并二氧磷杂环己烷（３ａ－３ｇ），用结晶法分离得到了７对非对映消旋体，其结构经ＨＮＭＲ、＾３１ＰＮＭＲ和元素分析确证，化合物３ａ－Ａ单晶Ｘ射线分析表明其构型为（２Ｒ，４Ｓ；２Ｓ，４Ｒ），生物活性测定结果表明，化合物３ｃ有良好的杀虫活性，非对映消旋体Ａ和Ｂ具有协同杀虫作用。     

氟代碳核苷类化合物的合成研究──N－烷基－5－甲酰胺基－1，2，4－氧杂二唑基－3－（4＇－脱氧－4＇－氟－β－L－吡喃型阿拉伯糖）的合成

报道了Ｎ－烷基５－甲酰胺基－１，２，４－氧杂二唑基－３－β－Ｄ－吡喃木糖用二乙胺基三氟化硫选择性氟化，得到相应的Ｎ－烷基－５－甲酰胺基－１，２，４－氧杂二唑基－３－（４＇－脱氧－４＇－氟－β－Ｌ－吡喃型阿拉伯糖）；并用光谱分析确证了它们的构型及在溶液中的构象。     

5—甲基—2—巯基—1,3,4—噻二唑的合成

５－甲基－２－巯基－１，３，４－噻二唑的合成李占才李淑勉方少明侯守君聂晓兵林烨（郑州轻工业学院化工系郑州４５０００２）关键词５－甲基－２－巯基－１，３，４－噻二唑乙酰肼Ｎ－乙酰肼基二硫代甲酸钾中图分类号Ｏ６２６．２７５－甲基－２－巯基－１，３，４－噻...     

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.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

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.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

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.