3-叠氮-4-氨基呋咱的合成及其晶体结构

以乙二醛和盐酸羟胺为原料,经加成,闭环和氮化反应制备了新型含能化合物3-叠氮-4-氨基呋咱(AAF),其结构经NMR,IR,X-射线单晶衍射仪及元素分析表征。AAF晶体属单斜晶系,P21/c空间群,晶胞参数为:a=0.5329(16)nm,b=1.0722(3)nm,c=0.8492(2)nm,α=90.00°,β=99.03(2)°,γ=90.00°,V=0.5046(2)nm3,Dc=1.660g.cm-3,Z=4,F(000)=256,μ(MoKα)=0.138mm-1。最终偏离因子R1=0.0768,wR2=0.1983。AAF晶体存在分子间氢键。     

2-叠氮基-1,1-二硝基乙基取代苯衍生物的合成

详细研究了2-叠氮基-1,1-二硝基乙基取代苯衍生物的合成方法。由苯基二硝基甲烷钾盐经羟甲基化,磺酰酯化和叠氮化得到目标化合物:3-硝基-(2-叠氮基-1,1-二硝基乙基)苯(4b),4-硝基-(2-叠氮基-1,1-二硝基乙基)苯(4c),m-二(2-叠氮基-1,1-二硝基乙基)苯(10)和p-二(2-叠氮基-1,1-二硝基乙基)苯(15)。     

2,5-二溴-4-硝基咪唑的合成

以咪唑为原料,经硝化和溴化反应合成了抗炎药物中间体——2,5-二溴-4-硝基咪唑,总收率80.3%,其结构经1H NMR和IR确认。     

Synthesis and Characterization of Some N-Aryl-4-nitroimidazoles as Potential Insensitive Energy Materials

N‐Aryl derivatives of 4‐nitroimidazole have been synthesized under CuI/TBAB catalytic system in excellent yields, using KOH as base in DMF solvent.     

1—烷基—2—甲基—4—硝基咪唑类化合物的合成及生物活性

利用固－液相转移催化法合成了７种α，ω－双［１－（２－甲基－４－硝基咪唑基）］烷烃和２０种１－烷基－２－甲基－４－硝基咪唑类化合物，大多数化合物收率在８５％以上。初步生物活性试验结果表明，部分化合物具有一定的抗炎、抗菌、镇痛、镇静或抗脑缺氧活性。     

3-叠氮基-4-酰氯肟基呋咱的合成及其热稳定性

以3-氨基-4-酰氨肟基呋咱为原料,经重氮化和叠氮化反应合成了新化合物3-叠氮基-4-酰氯肟基呋咱(3),总收率67％.其结构经1H NMR,13C NMR,15N NMR,IR及元素分析表征.热失重法研究结果表明,3具有良好的热稳定性.     

邻羟基α-叠氮苯乙酮衍生物的合成

以邻羟基苯乙酮衍生物为原料,经溴化反应和叠氮化反应合成了一系列邻羟基α-叠氮苯乙酮衍生物,其结构经1H NMR,13C NMR,IR及HR-MS表征.     

可能用于光动力诊疗的2-硝基咪唑卟啉衍生物的合成及表征

从吡咯和对羟基苯甲醛等起始原料出发,设计合成了4种具有潜在肿瘤乏氧检测及光动力治疗作用的2-硝基咪唑修饰新型卟啉衍生物.目标化合物结构经紫外、红外、质谱和核磁确证.     

Synthesis of New Substituted 4-Amino-3,5-dinitropyridine Derivatives

Facile synthetic routes for the preparation of some new 4-amino-3,5-dinitropyridine derivatives have been revealed. Nitration of 2-chloropyridin-4-amine （1） as a starting material, in an unexpected one-step reaction, to give dinitrated derivatives, followed by nucleophilic substitution reactions with sodium azide, potassium fluoride, ammonia, methylamine, and 4-nitroimidazol, respectively, gave substituted 4-amino-3,5-dinitropyridine derivatives. Meanwhile, its azide derivative underwent a ring closure conversion into 7-amino-6-nitro-[1,2,5]oxadiazolo[3,4-b]- pyridine-1-oxide. It is of significance that all of the nucleophilic substitution reactions were carried out under mild conditions.     

3-氨基-4-氨基肟基呋咱的合成及其晶体结构

以丙二腈为原料,用一锅法合成了呋咱类含能化合物3-氨基-4-氨基肟基呋咱(AAOF),收率72.4%。用1H NMR,13C NMR,IR,MS,元素分析和四圆单晶X-射线衍射仪对其分子和晶体结构进行了表征。结果表明:AAOF晶体属单斜晶系,空间群P21/c。主要晶体结构参数为:a=0.7651(3)nm,b=1.1702(3)nm,c=1.9216(10)nm,β=96.47(4)°,V=1.7095(12)nm3,Z=12,Dc=1.668 g.cm-3,F(000)=888。AAOF分子共面性较好,晶体中存在分子内和分子间氢键。     

N‐Nitrosarcosine: An Economic Precursor for the Synthesis of New Energetic Materials

New energetic compounds have been synthesized starting from the readily available N‐(cyanomethyl)‐N‐methylamine. From this, N‐nitrosarcosine was prepared in few steps, which serves as a starting material for the synthesis of oxygen‐rich compounds. The compounds were thoroughly characterized including multinuclear NMR and vibrational spectroscopy and also molecular structures by single X‐ray diffraction were obtained. Their energetic properties were determined including the sensitivities towards impact and friction, their heat of formations were calculated and the detonation and combustion parameters were predicted using EXPLO5 V6.02.     

Synthesis,characterization and theoretical study of 2-azido-4- nitroimidazole-based energetic salts

The 2-azido-4-nitroimidazole-based energetic salts were synthesized in a simple and straightforward manner. The structures of these new salts were determined by IR, 1H NMR and 13C NMR spectroscopy and elemental analysis. These salts also exhibited high positive enthalpies of formation, high nitrogen content, and moderate detonation properties.     

Synthesis,Characterization and Thermal Behaviors of 4-Amino-5-nitro-1,2,3-triazole(ANTZ)and Its Derivatives

4‐Amino‐5‐nitro‐1,2,3‐triazole (ANTZ) and its derivatives, such as 2‐(4‐amino‐5‐nitro‐1,2,3‐trazole‐1‐yl)‐1,3,5‐trinitrobenzene (T‐ANTZ) and 4‐amino‐5‐nitro‐1,2,3‐triazole (M‐ANTZ), were synthesized and characterized, whose structures were confirmed by IR, NMR and elemental analysis. The thermal behaviors of ANTZ, T‐ANTZ and M‐ANTZ were studied by the methods of DSC and TG‐DTG, and the results showed that there is an obvious melting process of ANTZ with melting point of 278.38°C, while there is no melting process in the thermal behavior of T‐ANTZ and M‐ANTZ (the derivatives of ATNZ).     

3,4-二氨基呋咱基氧化呋咱的合成及其晶体结构

通过3-氨基-4-氯肟基呋咱在稀碱作用下发生脱HC l,1,3-偶极反应制备了新型呋咱(氧化呋咱)类含能化合物3,4-二氨基呋咱基氧化呋咱(DAFF),产率70%。其结构经NMR,IR,四圆单晶X-射线衍射仪和元素分析表征。DAFF晶体属单斜晶系,空间群P21/c,a=0.8255(3)nm,b=0.9731(3)nm,c=1.1958(4)nm,β=91.93(3)°,Z=4,Dc=1.745 g.cm-3。DAFF分子不共面,三个环面扭曲。晶体中存在分子内和分子间氢键。     

4-羟基-2-吡啶酮类化合物的合成研究进展

4-羟基-2-吡啶酮是天然生物碱结构母核,同时也是一类重要的医药中间体,该类衍生物具有抗真菌、抗菌和抗肿瘤等多种生物活性.因此,其合成得到了广泛的研究和关注.综述了近年来4-羟基-2-吡啶酮类化合物的合成方法及其研究进展.     

含苯并噁唑基的硫桥杯[4]芳烃衍生物的合成及结构

在碳酸钾存在下, 对叔丁基硫桥杯[4]芳烃(1)分别与端基二溴代烷和碘甲烷反应, 生成硫桥杯[4]芳烃衍生物2～4. 含端基溴代的硫桥杯[4]芳烃衍生物2和4分别与2-巯基苯并噁唑在碳酸钾存在下反应, 生成硫桥杯[4]芳烃衍生物5a～5d. 通过1H NMR, 13C NMR, IR, MS和元素分析等手段对产物进行了表征. 同时, X射线分析确定了硫桥杯[4]芳烃5b的晶体结构.     

Synthesis and Crystal Structure of 4-Azido-2,2,6,6-Tetramethylpiperidine-1-oxyl Free Radical

1 INTRODUCTION Stable nitroxyl radicals are widely used in mole- cular biology, molecular pharmacology and phar- macy for noninvasive characterization of enzymes, receptors and drug delivery systems[1, 2]. They are al- so applied to examine the active center topography, the penetration of water, microviscosity, micropolo- rity, PH and oxygen concentration of their surroun- ding as well as spin carriers due to their exceptional stability and ease of chemical modification[3, 4]. However, th…     

2-取代-3-芳基-4-噻唑啉(硫)酮衍生物的合成、晶体结构和生物活性

从2-取代-3-芳基-4-噻唑啉酮(4a～4e和5)合成了三个系列新型噻唑啉酮衍生物, 即5-芳基亚甲基-4-噻唑啉酮(6a～6j), 4-噻唑硫酮(7a～7e和8)和4-氰基亚胺基噻唑烷(11a～11e和12). 中间体4a～4e和5由醛、胺和巯基乙酸缩合得到. 所有化合物的结构均经元素分析和¹H NMR确证, 并且采用X射线单晶衍射分析方法测定了化合物4b的结构. 初步生物活性试验结果表明, 部分标题化合物具有一定的杀菌活性和促进黄瓜子叶生根活性.     

Synthesis and Antibacterial Study of Novel Harmine Derivatives and Tetrahydro-β-Carboline Derivatives In Vitro

Dairy mastitis is a disease of dairy cattle caused by a variety of pathogenic microorganisms which has biought huge economic losses aused huge economic losses to the world. In this paper, Harmine derivatives and tetrahydro-β-carboline derivatives synthesized by the splice method are shown to have a good inhibitory effect on the pathogenic bacteria of dairy mastitis. The results of a bacteriostatic test on pathogenic bacteria of dairy cow mastitis (S. dysgalactiae, S. pyogenes, B. subtilis and P. vulgaris) showed that compound 7l had the best bacteriostatic effect on Streptococcus dysgalactiae, with a mic value of 43.7 μ g/mL. When the concentration of 7l was 1 × MIC and 2 × MIC, it had a significant inhibitory effect on Streptococcus dysgalactiae, and there was almost no growth of Streptococcus dysgalactiae at 4 × MIC. The binding properties of target compound 7l to amine oxidase [flavin-containing] A protein were simulated by the molecular docking technique. The ligand 7l achieved strong binding with the receptor through three hydrogen bonds. The hydrogen bonds were amino acid residues thr-52, arg-51 and ser-24, which are the main force for the compound to bind to active sites.     

四碘合汞酸银的合成及其在热致变色方面的应用

以硝酸汞、碘化钾和硝酸银为原料,在室温条件下,用液相法合成了四碘合汞酸银,并利用XRD谱和红外光谱技术对合成的四碘合汞酸银进行表征,证实了目标产物四碘合汞酸银已经形成。用扫描电镜技术观测四碘合汞酸银固体颗粒的形貌。然后采用一定方法,将合成的四碘合汞酸银分散到有机玻璃中,制得到掺有四碘合汞酸银的有机玻璃复合材料,并对该复合材料进行了热致变色的研究,发现该材料热致变色温度为48℃,而且可逆变色性能好,在热致变色方面具有应用的前景。