2-(1-H-四唑)-4’-甲基联苯的合成

以2-氰基-4'-甲基联苯(Ⅱ)为原料,与氨基钠反应得到2-脒基-4'-甲基联苯(Ⅲ),该化合物与水合肼发生取代反应得到4'-甲基-[1,1'-联苯]-2-甲酰胺酰肼(Ⅳ),最后在酸性条件下与亚硝酸钠发生闭环反应得到2-(1-H-四唑)-4'-甲基联苯(Ⅰ),总收率达到81%,其结构经1HNMR和MS确证。     

Anticonvulsant Profiles of Certain New 6-Aryl-9-substituted-6,9-diazaspiro-[4.5]decane-8,10-diones and 1-Aryl-4-substituted-1,4-diazaspiro[5.5]undecane-3,5-diones

Synthesis and anticonvulsant potential of certain new 6-aryl-9-substituted-6,9-diazaspiro[4.5]decane-8,10-diones (6a–l) and 1-aryl-4-substituted-1,4-diazaspiro[5.5]undecane-3,5-diones (6m–x) are reported. The intermediates 1-[(aryl)(cyanomethyl)amino]cycloalkanecarboxamides (3a–f) were prepared via adopting Strecker synthesis on the proper cycloalkanone followed by partial hydrolysis of the obtained nitrile functionality and subsequent N-cyanomethylation. Compounds 3a–f were subjected to complete nitrile hydrolysis to give the respective carboxylic acid derivatives 4a–f which were cyclized under mild conditions to give the spiro compounds 5a–f. Ultimately, compounds 5a–f were alkylated or aralkylated to give the target compounds 6a–i and 6m–u. On the other hand, compounds 6j–l and 6v–x were synthesized from the intermediates 5a–f through alkylation, dehydration and finally tetrazole ring formation. Anticonvulsant screening of the target compounds 6a–x revealed that compound 6g showed an ED₅₀ of 0.0043 mmol/kg in the scPTZ screen, being about 14 and 214 fold more potent than the reference drugs, Phenobarbital (ED₅₀ = 0.06 mmol/kg) and Ethosuximide (ED₅₀ = 0.92 mmol/kg), respectively. Compound 6e exhibited an ED₅₀ of 0.019 mmol/kg, being about 1.8 fold more potent than that of the reference drug, Diphenylhydantoin (ED₅₀ = 0.034 mmol/kg) in the MES screen. Interestingly, all the test compounds 6a–x did not show any minimal motor impairment at the maximum administered dose in the neurotoxicity screen.     

高热稳定和低感度多环类含能材料的设计与合成（英）

发展具有高能、低感、高热稳定性的新型含能材料是人们一直追求的目标。本研究设计、合成了一系列基于四唑连4,8-双呋咱并[3,4-b,e]吡嗪（DFP）的含能离子盐。含能离子盐具有优异的综合性能,如热分解温度较高（T_d：> 260 ℃）,感度较低（IS≥ 20 J,FS≥360 N）和爆速较高等（D > 8800 m·s^-1）。值得特别指出的是,化合物4e的热分解温度高达314 ℃,并且其爆速及撞击感度分别为9005 m·s^-1和25 J,是一种极具潜力的钝感高能量密度材料。     

Structural and Thermal Characterization of A Novel High Nitrogen Energetic Material: (NH4)2DNMT

1,4‐Dihydro‐5H‐(dinitromethylene)‐tetrazole ammonium salt ((NH₄)₂DNMT), a high nitrogen energetic compound, was synthesized and structurally characterized by single‐crystal X‐ray diffraction. The thermal behavior of (NH₄)₂DNMT was studied with DSC and TG‐DTG methods. The kinetic equation of the thermal decomposition reaction is: dα/dT=10^13.17/3β(1−α)⁻² exp(−1.388×10⁵/RT). The critical temperature of thermal explosion is 182.7 °C. The specific heat capacity of (NH₄)₂DNMT was determined and the molar heat capacity is 301 J mol⁻¹ K⁻¹ at 298.15 K. The adiabatic time‐to‐explosion of (NH₄)₂DNMT was calculated to be 277 s. The detonation velocity and detonation pressure were also estimated. All results showed that (NH₄)₂DNMT presents good performance.     

1-磺甲基四氮唑-5-硫醇双钠盐的合成

研究了头孢尼西的侧链１－磺甲基四氮唑－５－硫醇双钠盐的合成。以亚硫酸氢钠、甲醛、氨水为原料，经五步反应可制备１－磺甲基四氮唑－５－硫醇双钠盐，五步反应总收率为１０．８％ 。在原文献的基础上，作了一些改进，最主要的是第三步的烷基化试剂由溴乙烷替代碘甲烷，降低了工业成本，使本工艺易于工业化。     

含四唑环Schiff碱的合成与植物激素活性

以 5 氨基 1H 1 ,2 ,3,4 四唑与芳醛反应合成出五种新的Schiff碱 ,对其产率、物理性质、紫外光谱、红外光谱、质子的核磁共振谱及元素分析首次作了讨论 ,初步的生物活性测试试验证明 ,此类Schiff碱表现出显著的植物激素活性 ,一些化合物的生长素活性与生根性能优良。     

1-磺酸甲基-5-巯基四唑双钠盐的合成

综述、对比了1-磺酸甲基-5-巯基四唑双钠盐的合成工艺路线,提出了改进的、适于工业化的制备工艺。     

Synthesis and structural characterization of two novel 2D coordination polymers [PbCl(atza)]n and [PbCl(a4-ptz)]n

Reactions of Katza (atza⁻ = 5-aminotetrazole-1-acetato) or Ka4-ptz (a4-ptz⁻ = 5-[N-acetato(4-pyridyl)]tetrazole) with PbCl₂in aqueous solution, produced two new Pb(II) compounds, [PbCl(atza)]_n (1) and [PbCl(a4-ptz)]_n (2). Both compounds were structurally characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. In 1 or 2, the Pb(II) centers are connected through the atza⁻ or a4-ptz⁻ bridging ligand to form a two-dimensional layered structure. The luminescence properties of 1 and 2 were investigated at room temperature in the solid state.     

国外四嗪四唑类高氮含能材料研究进展

对国外正在研究的四嗪、四唑类高氮含能材料进行了综述,介绍了部分四嗪、四唑类高氮化合物及其衍生物的合成、理化性质和应用前景,对国外研究的3,6-二肼基-1,2,4,5-四嗪(DHT)、3,3′-偶氮(6-氨基-1,2,4,5-四嗪)(DAAT)、3,6-双(1氢-1,2,3,4-四唑-5-氨基)-1,2,4,5-四嗪(BTATz)、联四唑(BHT)等进行了重点描述。