1,9—二叠氮基—2,2,8,8—四硝基—4,6—二氧杂壬烷的合成及性能

１，９－二叠氮基－２，２，８，８－四硝基－４，６－二氧杂壬烷的合成及性能阎红＊管晓培（北京工业大学化学与环境工程学系北京１０００２２）（北京理工大学化工与材料学院北京）关键词叠氮化合物，含能增塑剂，合成，离去基团，性能评价１９９６－０９－２３收稿，１...     

N，N＇－双（2－硝基－苯并二氧化呋咱）－3，5－二硝基－2，6－二氨基吡啶的合成

Ｎ，Ｎ＇－双（２－硝基－苯并二氧化呋咱）－３，５－二硝基－２，６－二氨基吡啶的合成王乃兴，陈博仁，欧育湘　　　　　　　　　（北京理工大学化工与材料学院北京１０００８１）含能材料的研究，已在杂环领域取得了重大进展，杂环特别是氮杂环含能材料，具有密度高，...     

2，4－二硝基和二氰基高立方烷的合成

２，４－二硝基和二氰基高立方烷的合成管晓培，杜建卫，孙建光，于永忠（北京理工大学化学工程与材料学院北京１０００８１）关键词高立方烷，硝基，氰基，氧化近年来，作为新型的高能量密度材料，含能多面体烷衍生物的合成引起人们极大兴趣［１～３］。高立方烷的张力能...     

2－氯／2－甲磺酰基－5－（2－苯基－4－喹啉基）－1，3，4－噁二唑化合物的合成及其亲核取代的研究

借处理２－羟基－５－（２－苯基－４－喹啉基）－１，３，二唑同ＰＣｌ＿５／ＰＯＣｌ＿３之间的反应合成了２－氯－５－（２－苯基－４－喹啉基）－１，３，４－二唑（３）和通过２－基－５－（２－苯基－４－喹啉基）－１，３，４－二唑的甲基化，然后氧化制得２－甲磺酰基－５－（２－苯基－４－喹啉基）－１，３，４－二唑（６）．并分别研究了３和６同胺、叠氮及肼的反应，得到２，５－二取代的二唑新衍生物．初步观察了部分化合物的抗菌活性．     

二和四叠氮化合物的合成

由一,二和三乙二醇二（２－氯乙酸酯）,Ｎ,Ｎ’－１,２－亚苯基二９２－氯乙酰胺）和季戊四醇四（２－氯乙酸酯）分别与０．５ｍｏｌ／Ｌ ＮａＮ３的二甲基亚砜溶液于室温下反应１ｈ,可以高产率,高纯度地合成相应的二和四叠氮化合物。     

苯甲酸（1H－1，2，4－三唑－1－基）－3，3－二甲基－2－丁酮酯衍生物的合成

用冠醚作催化剂，通过苯甲酸盐同１－溴代－１－（１Ｈ－１，２，４－三唑－１－基）－３．３－二甲基丁酮－２－反应，合成了一系列苯甲酸（１Ｈ－１，２，４－三唑－１－基）－３，３－二甲基－２－丁酮酯类新化合物，并对合成方法进行了探讨。通过ＩＲ、￣１ＨＮＭＲ及元素分析，确定了化合物的结构。     

叠氮多硝基化合物的合成

在成功制备出含能增塑剂－1,11－二叠氮基－2,2,10,10－四硝基－5,7－二氧杂－十一烷的基础上,我们合成出它的一些衍生物,如1,1,1,9,9,9－六硝基－4,6－二氧杂－壬烷,1,4－二叠氮基－2－,2－二硝基丁烷,5,5－二硝基1,3－二氧杂－环庚烷和1－叠氮基－3,3,3－三硝基丙烷,并讨论了它们的性质。     

α－羰基－α－（1H－1，2，4－三唑－1－基）乙烯基芳基酮衍生物的合成及生物活性研究

α－（１Ｈ－１，２，４－三唑－１－基）取代苯乙酮与异硫氰酸苯酯在强碱条件下经缩合、卤化后得到含三唑的烯酮氮硫缩醛化合物１．该化合物与各种卤代物反应，形成了包括五元、六元杂环的缩合产物。部分结构具有一定的植物生长调节活性。     

2－羟基2＇烷氧基－1，1＇－联萘化合物的~1HMNR研究

研究了２－羟基－２＇－异丙氧基－１。１－联萘（３）等联萘化合物的~１ＨＮＭＲ谱或ＣＯＳＹ谱。此类化合物因２及２＇位取代基不同，两个萘环上同位质子不再等价，萘环质子峰增至１２组。化合物３~１ＨＮＭＲ谱峰的归属表明，萘环环电流各向异性对另一萘环质子的屏蔽作用与作者早期研究结果［１］一致。２（或２＇）位取代基上的质子的化学位移也与另一萘环平面相对位置有关。     

4－芳氧基－4－氧代－1，3，4－二氮磷杂环戊－2－硫酮类化合物的合成及其除草活性

４－芳氧基－４－氧代－１，３，４－二氮磷杂环戊－２－硫酮类化合物的合成及其除草活性陈茹玉，张成祥，冯克胜，程慕如（南开大学元素有机化学研究所天津３０００７１）关键词二氮磷杂环戊硫酮，酚类化合物，除草活性前文［１，２］曾报道含膦脲五员环类化合物的合成，...     

Indole derivatives

The Fischer cyclization of arylhydrazones of 1-butyl-, 1-benzyl-, and 1-cyclohexyl-3-pyrrolidinones has been studied, as a result of which a synthesis of 1, 2,3,4-tetrahydropyrrolo[3,4-b]indoles has been developed. The structure of the compounds obtained has been confirmed by their UV and NMR spectra and by a number of chemical properties.     

A study of some 1-alkyl-2,3-dihydroimidazo[1,2-a]benzimidazoles

A series of 1-alkyl-7-nitro (and 7-amino)-2,3-dihydroimidazo[1,2-α]benzimidazoles has been prepared. Similarly, a series of 1-alkyl-2,3-dihydroimidazo[1,2-α]benzimidazoles has been prepared. The prototropic tautomerism of this system has been studied. The site of electrophilic attack (alkylation) has been examined. 1-Alkylation takes place under strongly basic conditions and 9-alkylation occurs under neutral conditions.     

Determination of cadmium and copper with ET-AAS after electrochemical deposition on a graphite electrode

The electrodeposition of cadmium and copper on a special graphite disk electrode has been performed at controlled potential. The electrode with the deposit has been inserted into the graphite atomizer HGA-400 by an adapted automatic sampler for the final determination by ET-ASS. The sensitivity of determination has been 0.371 (microg l(-1))(-1) for cadmium and 0.025 (microg l(-1))(-1) for copper for 2 min electrodeposition and increased linearly with the time of deposition. The limit of detection (3s(bl)) has been 7.9 ng l(-1) Cd(2+) and 0.11 microg l(-1) Cu(2+) for 2 min deposition and it has been improved with increased time of electrodeposition. The technique has been applied to the determination of both metals in seawater and to speciation in the presence of EDTA complexing agent.     

Hydroxylamine derivatives

The condensation of urethane and ethyl acetohydroximate with 2-chloromethyl-1-methylbenzimidazole has given, respectively, N-ethoxycarbonyl-O-(1-methylbenzimidazol-2-ylmethyl)hydroxylamine and ethyl N-(1-methylbenzimidazol-2-ylmethoxy)acetimidate. Acid hydrolysis of the latter has given O-(1-methylbenzimidazol-2-ylmethyl)hydroxylamine. The reactions of its derivatives with HCl have been studied, and it has been shown that 1-methylbenzimidazole-2-aldehyde O-(1-methylbenzimidazole-2-methyl)oxime is formed. The structure of the latter has been shown by an analysis of its PMR spectra.For part II, see ¦1¦.     

Polyamides from 12-(β-aminoethyl) abietan-18-amine

The 1:1 salt of 12-(β-aminoethyl)abietan-18-amine and adipic acid has been prepared and polymerized. This salt has been copolymerized with the 1:1 salt of hexamethylenediamine and adipic acid. 12-(β-Aminoethyl)abietan-18-amine has been polymerized with isophthaloyl and terephthaloyl chlorides with triethylamine as catalyst and terpolymerized with terephthaloyl chloride and hexamethylenediamine. All polymers have been characterized to some extent, and mechanical properties are reported for two of the polyamide films.     

1－甲氧基－1－锂乙烯的结构及其分解反应的DFT研究

用量子化学中的密度泛函DFT方法，在B3LYP／631G（d,p）水平上研究了－甲 氧基－1－锂乙烯的结构。结果表明，1－甲氧基－1－锂乙烯有4种平衡结构，其中 只有1种是稳定的。对稳定的平衡结构，找到了分解反应的过渡态。在得到分解反 应过渡态的基础上，根据Eyring过渡态理论，计算了不同温度下1-甲氧基－1-钾乙 烯分解反应的速率常数，并根据速率常数计算了其平均寿命τ，根据平均寿命τ讨 论这类物质的稳定性问题。     

Enzyme electrode probes obtained by electropolymerization of monomers with PMS and selected dehydrogenase enzymes

5-methylphenazonium methylsulphate, (commonly named phenazine methosulphate, PMS) mediated electroxidation of beta-nicotinamide adenine dinucleotide (phosphate), reduced form, (NAD(P)h), on platinum, gold and carbon electrodes has been studied by electropolymerization of 1,2-, 1,3-, 1,4-diaminobenzene (DAB), pyrrole-2-carboxylic acid (PY-2-COOH) and 4,4'-dihydroxybenzophenone (DHB) in presence of PMS using cyclic voltammetry. The electroxidation of ascorbic acid has been evaluated on the electrodes electropolymerized in absence and in presence of PMS. The same experiments have been carried out with NAD(P)H in solution. Results showed that the NAD(P)H is oxidised by PMS coimmobilized with the polymer film on the electrode surface. NAD(P)H has been measured in the range 10(-6)-10(-2)mol l(-1) with a detection limit of 5 x 10(-7) mol 1(-1). Amperometric measurements of NAD(P)H have been carried out at -0.10 V and the efficiency of different elecrodes based on different materials has been studied. The electropolymerization has been also carried out in presence of PMS and selected dehydrogenase enzymes. The activity of these enzymes has been tested amperometrically at -0.1 V. Enzyme substrates such as glucose, lactate and glutamate have been measured in the range 5 x 10(-6)-1 x 10(-2) mol 1(-1) with a detection limit 1 x 10(-6) mol 1(-1). Also the stability of these probes during time has been evaluated.     

Structure of 6-Epiforsticine and Revision of the Stereochemistry of Forsticine

In the course of our investigation on Aconitum and Delphinium species, we have isolated a number of norditerpenoid and diterpenoid alkaloids from A. kuzsnezoffii and A. hemsleyanum var. pengzhouense1~6. We have found that a norditerpenoid alkaloid, 6-epiforsticine isolated from both plants shows a great deal of similarity to forsticine7 but significantly differed from the latter in its 13C NMR spectrum (Table l), suggesting that the alkaloids were a pair of epimers at C-6. The present comm…     

Cycloaddition in Condensed Isoindoles. 2. Method for Obtaining New Derivatives of 2-Phenylpyridine

The reaction of pyrido[2,1-a]isoindole with maleimide derivatives has been investigated. A new rearrangement has been found, the products of which are 2-[2'-(1-R-2,5-dioxopyrrolidinidene)-2'-(1-R-2,5-dioxopyrrolidinyl)methyl]phenylpyridines. A probable mechanism for the rearrangement has been proposed. The existence of atropoisomerism for the compounds obtained has been demonstrated by ¹H NMR spectra.     

The copolymerisation of 2,4-dicyanobut-1-ene with N-vinyl carbazole

The copolymerisation of the monomers 2,4-dicyanobut-1-ene and N-vinyl carbazole has been studied. The presence of a charge transfer complex from these two monomers with a 1:1 stoichiometry has been established, and a value of 0.22 dm³ mol⁻¹ at 298 K for the equilibrium constant for complex formation has been obtained from NMR measurements. The copolymer composition data have been analyzed allowing for the participation of the complex in the propagation reactions; the results have been compared with the predictions of two simpler terminal models and with the penultimate model.