2,6-二氨基-3,5-二硝基吡啶-1-氧化物的合成新方法

研究了2,6-二氨基-3,5-二硝基吡啶-1-氧化物(ANPyO)的合成新方法. 以2,6-二氨基吡啶为起始原料, 经酰基化、N-氧化、硝化三步反应得到ANPyO, 总收率为75%. 测试了ANPyO的爆速、爆压、DSC, 以及电火花感度和落锤感度, 同1,3,5-三氨基-2,4,6-三硝基苯(TATB)的性能进行了对比, 结果表明ANPyO综合性能和TATB基本相当. 用1H NMR, MS和红外光谱对ANPyO及其中间体结构进行了表征.     

3-氯-4-二苄胺基-5-甲氧基-2(5H)-呋喃酮的合成与晶体结构

在THF溶液中合成了标题化合物3-氯-4-二苄胺基-5-甲氧基-2(5H)-呋喃酮,并用FT-IR、UV-Vis、1HNMR、13C NMR、MS、元素分析和X-射线衍射等进行了表征。结果表明此化合物属正交晶系,空间群为Pbca,晶胞参数为:a=15.891(16),b=11.126(11),c=19.778(19),α=β=γ=90°,V=3497(6)3,Z=8,Dc=1.306Mg/m3,μ=0.234 mm-1,F(000)=1440。在化合物的分子结构中,两个苯环几乎垂直于呋喃酮平面,且它们与呋喃酮平面的两面角分别为89.38°和88.19°。     

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

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.     

2-甲氧基-3-氟-4-碘吡啶的合成

2-甲氧基-3-氟-4-碘吡啶是一个重要的医药化工中间体,其合成路线未见文献报道。以2-甲氧基-3-氟-5-氯吡啶为起始原料,经氢解和碘代两步反应合成标题化合物,总收率62.8%,其结构经¹H NMR, ¹³C NMR和MS确证。     

6-甲基-5-硝基-3-吡啶硼酸频哪酯合成工艺的改进

以2-氯-3-硝基-5-溴吡啶为起始原料,经取代反应、水解反应、Suzuki偶联反应得到6-甲基-5-硝基-3-吡啶硼酸频哪酯。反应总收率为51%,中间体及目标产物结构由IR和1H-NMR表征。     

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

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.     

2,6-二氨基-3,5-二硝基吡嗪-1-氧化物的合成

研究了2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105)的合成新方法. 该方法是以2,6-二氯吡嗪和甲醇钠作为起始原料, 经烷氧基化、硝化、胺化、N-氧化四步反应得到LLM-105, 总收率为50%. 用¹H NMR, ¹³C NMR, IR, MS和元素分析对LLM-105及其中间体结构进行了表征.     

3,5-二(吡啶-甲氧基)苯甲酸吡啶-甲基酯的合成

具有三脚架构型的多吡啶类化合物,因其具有众多的配位原子以及较为特殊的分子构型,在与金属离子配位的过程中,一方面可以通过吡啶氮的配位键、氢键、芳香环的π-π作用等方式构筑出结构新颖的配合物[1-4];另一方面因其具有三脚架的构型,其三条侧链可自由翻转形成大小合适的空腔,能够与不同的客体分子或离子结合,有可能筛选出在分子识别、分子交换、电子传递和选择性催化等方面具有特殊性能的功能材料[5-8].因此,合成具有三脚架构型的多吡啶类配体是这些配合物在诸多领域中应用的关键.     

一种有效制备2-氨基-3,5-二硝基-6-氯吡啶及其衍生物的方法

研究了2-氨基-3,5-二硝基-6-氯吡啶(4)及其衍生物的制备新方法.以廉价易得的2,6-二氯吡啶(1)为起始原料,通过硝化、氨化、硝化反应步骤得到中间体2-氨基-3,5-二硝基-6-氯吡啶(4),再与氨、叠氮化钠等亲核试剂反应分别得到2-氨基-3,5-二硝基吡啶-6-取代衍生物5~7.研究表明该方法具有原料便宜易得、后处理操作简单和产品纯度高等优点.     

2,6-吡啶二亚胺基锰(Ⅲ)配合物的合成、晶体结构及催化性能

由三齿含氮配体2,6-二[1-(2,6-二甲基苯基亚胺)乙基]吡啶(L1)、2,6-二[1-(2,6-二乙基苯基亚胺)乙基]吡啶(L2)和2,6-二[1-(2,4,6-三甲基苯基亚胺)乙基]吡啶(L3)分别与MnCl2·4H2O在乙腈中反应,合成了3个新的具有较大空间位阻的2,6-吡啶二亚胺基氯化锰配合物L1Mn(Ⅱ)...     

Synthesis and Crystal Structure of 2,6-Bis（2-pyridinylmethyl）-3,5-bis（2-hydroxyl-5-chlorophenyl）pyrazine

The title compound,2,6-bis(2-pyridinylmethyl)-3,5-bis(2-hydroxyl-5-chlorophe nyl)-pyrazine(C26H12Cl2N4O2C2H8O2,Mr=551.41),has been synthesized and characterized by LC-ESIMS,NMR,UV and IR spectroscopy as well as by X-ray single-crystal diffraction.The compound behaves as a substituted pyrazine.The hydrogen atoms on C(2) and C(3) are substituted by 2-pyridinyl,whereas those on C(1) and C(4) are substituted by 2-hydroxyl-5-chlorophenyl.It crystallizes in the monoclinic system,space group P21/c with a=8.9433(12),b=32.003(4),c=10.5209(18),β=111.199(2)°,V=2807.5(7)3,Z=4,Dc=1.305 mg/m3,F(000)=1144 and μ=0.094 mm-1.A total of 13235 reflections were collected in the range of 2.17～25.01o by using a phi and omega scan mode,of which 4923 were unique(Rint=0.0692) and 2872 observed reflections with Ⅰ > 2σ(Ⅰ) were used in the structure solution and refinement.     

Synthesis and Crystal Structure of 3,5-Dicyano-2,6-diethylthiopyridine

3,5-Dicyano-2,6-diethylthiopyridine has been synthesized by the alkylation of cyanothioacetamide with ethyl iodide in DMF and its molecular and crystal structures have been investigated. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1351–1354, September, 2005.     

Synthesis and Crystal Structure of 5-Diazo-4-ethoxycarbonyl-3-methylthio Pyrazol

1 INTRODUCTION It is reported that diazo pyrazoles are im- portant intermediates in the synthesis of numerous fused pyrazole heterocyclic compounds, which maybe exhibit high pharmaceutical functions and pesticidal activity[1]. So far, diazotization is a…     

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.     

Resolution of RS-3-chloro-2-oxy-propyltrimethylammonium-chloride and Crystal Structure Studies on Its R,R-tartrate

1 INTRODUCTION RS-3-chloro-2-oxy-propyltrimethylammonium-chloride 1 and its enantiomers were important inter- mediates. For example, S-(-)-1 is an intermediate of L-carnitine[1]; R-(+)-1 is an intermediate of optically pure acetylcholine[2]; and compound 1 has also been used in other ways[3, 4]. RS-3-chloro-2-oxy-propyltrimethylammonium-chloride 1 has been synthesized and resolved with R,R-tartric acid. Di-(S-3-chloro-2-oxy-propyltri- methylammonium)-R,R-tartrate 2 was obtained and …     

Synthesis and Crystal Structure of 2,3-Diethoxycarbonyl-4-phenyl-5-morpholinyl Thiophene

1INTRoDUCTIONa-Thiocarbonylthioformamidesweresynthesizedin198o[l~2i,however,thereisnoreportofthesecompoundsconcerningtheirpropertiesandreactionactivitiest33.Accordingtotheirstructure,theyseemtohavereactionwithdienophi1es,likesubsti-tutedolefinicandacetylenicdienophilestoleadcorrespondingDiels-Alderproduct.xylene(15ml),diethylbutynedioicester(O.2g,1.2mmol)wasadded,themix-turewasrefluxedfor20h,thencooledtoroomtemperatureandconcentrated.Theresiduewaspurifiedbysilicagelcolumnusingacetone/petr…     

Synthesis,Crystal Structure and Theoretical Calculation of [2-（2,6-Dioxacyclohexyl）-5-methoxylphenols]2

The title compound [2-（2,6-dioxacyclohexyl）-5-methoxylphenols]2 was synthesized by the reaction of 2-hydroxyl-3-methoxylbenzaldehyde and 1,3-propanediol in the presence of DMF-DMS adduct and characterized by IR spectrum, UV-Vis spectrum and X-ray crystallography. The title compound belongs to monoclinic, space group P21 with a = 9.8967（10）, b = 8.2240（9）, c = 13.3654（14） A^°, β= 90.016（2）°, C11H14O4, Mr = 210.22, V = 1087.8（2）A^°3, Z = 4, Dc = 1.284 Mg/m^3, F（000） = 448,μ = 0.098 mm^-1, the final R = 0.0300 and wR = 0.0761 for 2070 observed reflections with I 〉 2σ（I）. The molecules are connected via intermolecular O-H…O hydrogen bonds into a 2D network structure. Moreover, theoretical investigations of the title compound with HF/6-31G（d） method were performed, and its stability, frontier molecular orbital composition and Mulliken charge distribution were also discussed. The compound is a bis-molecule. The two molecules stay together and could not be separated. Two crystallographically independent molecules exist in an asymmetric unit. The bond lengths and bond angles of the two molecules are slightly different with each other.     

Synthesis and Crystal Structure of 4-Salicyli deneamino-3-methyl-1,2,4-triazol-5-thione

1 INTRODUCTION 3-Substituted-4-amino-1,2,4-triazol-5-thione is the key synthon in the formation of heterocyclic compound. As a bifunctional agent, it can react with various electrophilic reagents and its derivatives have been reported to show various biological activities to be employed as fungicide[1], micro- biocide[2, 3], bactericide[4], herbicides[5] and anti in- flammatory agents[6]. Furthermore, 3-substituted-4- amino-1,2,4-triazol-5-thione has potential electron donors. Though ma…