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一个简易的2,6-二氨基-3,5-二硝基吡啶-1-氧化物的合成方法 总被引:3,自引:0,他引:3
研究了2,6-二氨基-3,5-二硝基吡啶-1-氧化物(DADNP-1-O)的一个简易合成方法. 该方法是以2,6-二氨基吡啶(DAP)为原料, 利用两步法得到高纯度高产率的2,6-二氨基-3,5-二硝基吡啶, 再在三氟乙酸和双氧水作用下进行N-氧化反应得到DADNP-1-O, 总收率在90%以上, 并对主要反应影响因素进行了讨论, 经傅立叶变换红外光谱(FT2IR), 氢核磁(1H NMR), 碳核磁(13C NMR), 高效液相色谱(HPLC), 元素分析, DSC等方法对中间体和DADNP-1-O结构进行了表征. 相似文献
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含能配合物2,6-二氨基-3,5-二硝基吡啶-1-氧化物合钴(Ⅲ)的合成、晶体结构及催化性能 总被引:2,自引:0,他引:2
培养了含能配合物2,6-二氨基-3,5-二硝基吡啶-1-氧化物(ANPyO)合钴(Ⅲ)晶体,用X射线单晶衍射法测定了其分子结构。该配合物的分子式为[Co(ANPyO)3]。用DSC,TG-DTG技术对该配合物的热分解进行了研究,结果表明,该配合物的热分解由1个缓慢吸热峰和2个剧烈的放热峰组成,剩余残渣量为3.7277%。感度测试结果表明,该配合物感度较ANPyO有一定程度的降低,是一种不敏感含能材料。同时研究了配合物对高氯酸铵(AP)热分解的影响,结果表明,[Co(ANPyO)3]可以使AP的高温分解峰温提前65.15℃,使分解速度加快,对AP热分解具有良好的催化效果。 相似文献
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合成了三种不同链长的1,ω-二(2-氨基吡啶)烷烃,分别为二溴化1,4-二(2-氨基吡啶)丁烷(C4)、二溴化1,6-二(2-氨基吡啶)己烷(C6)、二溴化1,8-二(2-氨基吡啶)辛烷(C8).考察了八元瓜环(Q[8])与上述三种1,ω-二取代烷烃的主客体相互作用,运用1H NMR及UV-vis证明三种客体与Q[8]的作用模式均不相同.在此基础上,考察了八元瓜环对三种底物光致环加成反应的超分子催化性能.结果表明,由于三种底物与Q[8]的主客体作用模式不同,八元瓜环对它们光二聚反应的超分子催化性能也各有差异. 相似文献
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吡啶-2,6-二甲酸与2,6-二氨基吡啶质子转移化合物的超声合成新方法 总被引:1,自引:0,他引:1
研究了超声波作用下合成吡啶-2,6-二甲酸(pydc·H2)与2,6-二氨基吡啶(pyda)质子转移化合物[pyda·H2]2+[pydc]2-的新方法,考察了不同溶剂、反应时间和反应物浓度等因素对产率的影响.结果表明,在较短时间的超声波作用下,于不同种类的溶剂中均可合成得到[pyda·H2]2+[pydc]2-.该合成方法操作简便,无需催化剂和加热,反应时间短,产率高,具有实用性. 相似文献
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First-principle calculations are performed on the dimers of 2,6-diamino-3,5-dinitropyridine (ANPy) and its N-oxide (2,6-diamino-3,5-dinitropyridine-1-oxide, ANPyO). The dimers as well as the monomers are fully optimized by the DFT-B3LYP and HF methods in conjunction with 6-311G**, 6-311++G**, and cc-pVDZ basis sets. The N-O bond length of the pyridine N-oxide moiety decreases in the ANPyO dimer in the dimerization process, which results in a larger deformation energy of the ANPyO submolecule. This deformation prevents the submolecules from further close contact and the formation of strong H-bonds between the nitro and amino groups. The optimized intermolecular distances of the ANPyO dimer are in good agreement with the corresponding experimental values. There is a weak C-H...O hydrogen bond in the ANPyO dimer; the B3LYP method underestimates its binding energy. On the contrary, for the ANPy dimer, the binding energy obtained at the B3LYP level is larger than that obtained at the HF level. The individual O...H strength is stronger in the ANPy dimer than that in ANPyO, which is consistent with the O...H distance. The O...H-C type of the H-bond is stronger in the ANPyO dimer than the ordinary O...H-C bond due to the N-oxide oxygen atom bearing larger negative charges. The corrected binding energy for each hydrogen bond between nitro oxygen and amino hydrogen is about −5 kJ/mol in the ANPy dimer, which is stronger than that in the ANPyO dimer. 相似文献
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以丙酮和甲酸乙酯为原料, 在醇钠的作用下合成了1,3,5-三乙酰基苯(1). 1与二溴新戊二醇在酸的作用下发生缩酮化反应, 制成1,3,5-三-(1-甲基-2,6-二氧杂-4,4-二溴甲基环己基)苯(2). 2与5,5-二甲基-4,6-二氧杂-1,3-环己二酮在乙醇钠的作用下合成了1,3,5-三-[7-(7-甲基-2,2-二-乙氧羰基-6,8-二氧杂螺[3.5]-壬基)]苯(3). 将3在氯仿中与季戊四醇进行酯交换反应得到产物1,3,5-三-[7-(7-甲基-2,2-二-(2,2-二羟甲基-3-羟基丙氧基羰基)-6,8-二氧杂螺[3.5]-壬基)]苯(4). 收率为47.7%. 标题化合物及中间产物使用IR, 1H NMR和MS或元素分析进行了表征. 相似文献
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A highly selective synthesis of 2,6-dimethylnaphthanlene(2,6-DMN) by transalkylation between 2-methylnaphthanlene(2-MN) and 1,2,4,5-tetramethylbenzene(TeMB) was performed with 1-alkyl-3-methylimidazo- lium aluminum chloride([Cnmim]Cl-AlCl3) ionic liquids(ILs) as catalysts. The influences of the alkyl group as the organic cation, the acidic strength of [C4mim]Cl-AlCl3 ILs as well as the reaction conditions on the catalytic performance were investigated. [C4mim]Cl-AlCl3 ILs[x(AlCl3)=71%] exhibited high activity and selectivity toward 2,6-DMN. The selectivity to 2,6-DMN and the 2,6-DMN/2,7-DMN ratio reached up to 68.2% and 3.7:1, respectively. The UV-Vis spectrum of TeMB treated by different ILs shows that the protonated degree of TeMB dependeds on the acidity strength of ILs, which has a significant impact on the reaction results. The high protonated degree of TeMB is advantageous to enhancing the conversion of transalkylation and the large stereo-hindrance effect of TeMB is favorable to improving the selecivity to 2,6-DMN. 相似文献
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以2-溴代-3-甲基环己酮和2-溴代-5-甲基环己酮混合物及2-甲基苯硫酚为原料,经耦合、环化及纯化制得1,2,3,4-四氢-2,6-二甲基二苯并噻吩(3);3在三氟乙酸中经锌粉还原合成了1,2,3,4,4a,9b-六氢-2,6-二甲基二苯并噻吩(4).3和4的结构经1H NMR,13C NMR和GC-MS确证. 相似文献
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1-(2,6-二氯-4-三氟甲基苯基)-3-氰基-5-氨基吡唑及其酰胺、二酰亚胺的合成及晶体结构 总被引:3,自引:0,他引:3
2,6-二氯-4-三氟甲基苯胺经重氮化后与2,3-二氰基丙酸酯反应合成了1-(2,6-二氯-4-三氟甲基苯基)-3-氰基-5-氨基吡唑(1), 1与乙酸酐、顺丁烯二酸酐、苯甲酰氯反应得到1的乙酰胺2a、顺丁烯酰亚胺2b和苯甲酰胺2c. 通过元素分析、红外光谱、核磁共振氢谱、核磁共振碳谱、质谱等手段对其结构进行了表征. 用X射线单晶衍射测定了化合物2a, 2b和2c的晶体结构. 2a属于单斜晶系, C2/c空间群, 晶胞参数a=1.88282(6) nm, b=0.86541(3) nm, c=1.90766(6) nm, β=95.5830(10)°, V=3.09362 nm3, Z=8, R=0.064, wR=0.170. 2b属于单斜晶系, P21/n空间群, 晶胞参数 a=1.28261(10) nm, b=0.89942(7) nm, c=1.46896(12) nm, β=104.217(1)°, V=1.6427(2) nm3, Z=4, R=0.055, wR=0.165. 2c属于三斜晶系, P-1空间群, 晶胞参数a=0.84613(11) nm, b=0.98923(13) nm, c=1.14305(15) nm, β=96.002(2)°, V=0.9326 nm3, Z=2, R=0.0684, wR=0.1795. 相似文献
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Therearemanykindsofhairdyeswithdifferentformulae.Thekindwedeterminedcontainsthefollowingfiveconstituentsfl,4-phenylenediamine(P-PDA),4-aminophenol(P-APO),3-aminophenol(m-APO),1,3-benzendiol(m-BDO)and2,6-diaminopyridine(DAP).Withreversed-phasehigh-performanceliquidchromatography(RP-HPLC),someotherkindsofhairdyeshadbeendetermined"',butnotourkind.lnthispaperwedescribeaRP-HPLCmethodsuitabIefortheseparationandquantitativedeterminationofallthosefiveconstituentsinhairdyes.Analyseswereperf… 相似文献