1,6‐Dinitroperylene Bisimide Dyes: Synthesis,Characterization and Photophysical Properties

1,6‐ and 1,7‐regioisomers of dinitro‐substituted perylene bisimides ( 1a — 1b and 2a — 2b ) were synthesized under mild condition in high yields. The 1,6‐ and 1,7‐regioisomers were successfully isolated from the regioisomeric mixture using conventional methods of separation and subsequently characterized by 500 MHz ¹H NMR spectroscopy. This is the first time when 1,6‐dinitroperylene bisimides ( 1a — 1b ) are obtained in pure form. Furthermore, the photophysical and electrochemical properties of 1 and 2 were found to be almost the same. The nitro functionalities provide stability of n‐type charge carriers by lowering the LUMO to resist ambient oxidation, which may offer potential applications in air‐stable n‐type organic semiconductors.     

含1,6-二氢-6-哒嗪酮的1,3,4-噁二唑啉和噻唑烷-4-酮类化合物的合成

以1,6-二氢-6-哒嗪酮-3-甲酰肼(1)与芳香醛反应得到相应的1,6-二氢-6-哒嗪酮-3-羰基芳香醛腙(2a～2e). 再将2a～2e与乙酸酐作用, 合环得到一系列含有1,3,4-噁二唑啉环的衍生物3a～3e; 在DMF中用HSCH₂COOH合环, 得到含有4-噻唑烷酮的衍生物4a～4e. 所有化合物的结构均经元素分析, IR, ¹H NMR 和MS谱得以证实.     

一种新型含萘聚醚酰亚胺的合成与表征

本文合成了一种新型含萘酰亚胺六元环结构的双氯单体BCNPI, 然后将其与双酚A双钠盐在环丁砜中高温缩聚, 得到一种新型含萘聚醚酰亚胺, 并对其基本性能进行表征.     

新型柔性配体1,6-二(1-苯并咪唑基)己烷的合成及表征

本文报道了含两个结晶水的高柔性二齿配体1,6-二(1-苯并咪唑基)己烷(HBBIm·2H2O)的合成、红外光谱、核磁氢谱、晶体结构和理论化学计算.这种新型的含氮和芳香环的高柔性配体通过分子间的O-H…O,O-H…N,C-H…π和π…π弱作用力形成三维网状超分子结构.量子化学计算结果表明,配体HBBIm上所有氮原子都有较多负电荷,有利于金属离子进行配位.     

Synthesis of 1,6-anhydro sugars catalyzed by silica supported perchloric acid

A new and efficient method for the preparation of 1,6-anhydro sugars using silica supported perchloric acid as a catalyst is described. The catalyst is heterogeneous and 1,6-anhydro sugars could be formed within a few minutes with good yields.     

Synthesis, Crystal Structure, and IR Spectroscopic Characterization of 1,6-Hexanediammonium Dihydrogendecavanadate

Summary.  Anhydrous 1,6-hexanediammonium dihydrogendecavanadate ((HdaH₂)₂H₂V₁₀O₂₈, 1) was prepared by reaction of V₂O₅ with 1,6-hexanediamine in aqueous solution. The crystal structure of 1 was determined, and the proton positions in the H₂V₁₀O₂₈ ⁴⁻ anion were calculated by the bond length/bond number method. The protons are bound to the centrosymmetrically oriented μ–OV₃ groups of the decavanadate anion. Based on the analysis of IR spectra of 1 prepared from H₂O and D₂O, the absorption band at 871 cm⁻¹ can be attributed to δ(V–O_b–H) vibrations. Received August 3, 2001. Accepted (revised) October 8, 2001     

Synthesis, Crystal Structure, and IR Spectroscopic Characterization of 1,6-Hexanediammonium Dihydrogendecavanadate

 Anhydrous 1,6-hexanediammonium dihydrogendecavanadate ((HdaH₂)₂H₂V₁₀O₂₈, 1) was prepared by reaction of V₂O₅ with 1,6-hexanediamine in aqueous solution. The crystal structure of 1 was determined, and the proton positions in the H₂V₁₀O₂₈ ⁴⁻ anion were calculated by the bond length/bond number method. The protons are bound to the centrosymmetrically oriented μ–OV₃ groups of the decavanadate anion. Based on the analysis of IR spectra of 1 prepared from H₂O and D₂O, the absorption band at 871 cm⁻¹ can be attributed to δ(V–O_b–H) vibrations.     

Synthesis and Crystal Structure of 5-Amino-7-benzylseleno-8-cyano-3-ethoxycarbonyl-4-(2-furyl)-1,2-dimethyl-1,4-dihydro-1,6-naphthyridine

5-Amino-7-benzylseleno-8-cyano-3-ethoxycarbonyl-4-(2-furyl)-1,2-dimethyl-1,4-dihydro-1,6-naphthyridine was obtained by N-alkylation. X-ray crystallography showed the presence of two symmetrically conformers in the crystal.     

4,4＇-二硝基二苯乙烷(烯)的合成

二硝基二苯乙烯;硝基甲苯;氧化二聚反应;4;4＇-二硝基二苯乙烷(烯)的合成     

3-芳基-6-甲基-1,6-二氢-1,2,4,5-四嗪及其衍生物的合成和晶体结构

以乙腈和芳基腈为原料, 经过醚化、环化和还原三步方便且有效地合成了3-芳基-6-甲基-1,6-二氢-1,2,4,5-四嗪, 并在此基础上合成了一系列新的3-芳基-6-甲基-1,6-二氢-1,2,4,5-四嗪衍生物, 通过元素分析, ¹H NMR, IR和HRMS对这些化合物进行了表征. 对化合物N-邻甲基苯-3-苯基-6-甲基-1,6-二氢-1,2,4,5-四嗪-1-甲酰胺(5a)的X射线晶体衍射研究表明: 其属于单斜晶系, P2_{1 /c空间群, 晶胞参数a＝1.3941(6) nm, b＝0.5675(2) nm, c＝2.0614(8) nm; α＝γ＝90°, β＝102.055(6)°; V＝1.5949(11) nm³, 此类化合物的四嗪环采用不对称船式结构, 且具有同芳香性.}     

Design,Synthesis and Biological Activities of Novel Benzoyl Hydrazines Containing Pyrazole

In search of environmentally benign compounds with high biological activity, low toxicity and low resistance, 8 novel benzoyl hydrazines containing pyrazole were designed and synthesized. All compounds were characterized by ¹H NMR spectra and HRMS. The preliminary results of biological activity assessment indicated that most of title compounds exhibited certain insecticidal activities against Mythimna separata Walker at 200 mg·L^?1 but excellent fungicidal activities against six fungus at 50 mg·L^?1, which were better than the control.     

Synthesis and properties of polyimides derived from 1,6-bis(4-aminophenoxy)naphthalene and aromatic tetracarboxylic dianhydrides

1,6-Bis(4-aminophenoxy)naphthalene ( I ) was used as a monomer with various aromatic tetracarboxylic dianhydrides to synthesize polyimides via a conventional two-stage procedure that included ring-opening polyaddition in a polar solvent such as N,N-dimethylacetamide (DMAc) to give poly(amic acid)s, followed by thermal cyclodehydration to polyimides. The diamine ( I ) was prepared through the nucleophilic displacement of 1,6-dihydroxynaphthal-ene with p-chloronitrobenzene in the presence of K₂CO₃, followed by catalytic reduction. Depending on the dianhydrides used, the poly(amic acid)s obtained had inherent viscosities of 0.73–2.31 dL/g. All the poly(amic acid)s could be solution cast and thermally converted into transparent, flexible, and tough polyimide films. The polyimide films had a tensile modulus range of 1.53–1.84 GPa, a tensile strength range of 95–126 MPa, and an elongation range at break of 9–16%. The polyimide derived from 4,4′-sulfonyldiphthalic anhydride (SDPA) had a better solubility than the other polyimides. These polyimides had glass transition temperatures between 248–286°C (DSC). Thermogravimetric analyses established that these polymers were fairly stable up to 500°C, and the 10% weight loss temperatures were recorded in the range of 549–595°C in nitrogen and 539–590°C in air atmosphere. © 1995 John Wiley & Sons, Inc.     

3,4-双取代氧化呋咱衍生物的合成、结构表征及热性能研究

以自制的偕氯肟基化合物为原料, 通过脱氯化氢、分子间二聚环化及硝化等反应合成了自行设计的8种目标化合物--3,4-二苯基氧化呋咱(1)、3,4-二(吡啶-2 -基)氧化呋咱(2)、3,4-二(吡啶-3 -基)氧化呋咱(3)、3,4-二(吡啶-4 -基)氧化呋咱(4)、3,4-二(吡嗪-2 -基)氧化呋咱(5)、3,4-二(4 -甲氧基苯-1 -基)氧化呋咱(6)、3,4-二(4 -氯苯-1 -基)氧化呋咱(7)及3,4-二(3 ,5 -二硝基苯-1 -基)氧化呋咱(8). 利用红外光谱、核磁共振、质谱、元素分析等手段对8种目标化合物进行了结构表征. 初步考察了不同取代基对二聚反应的影响, 发现取代基的吸电子能力越强, 越有利于形成氧化氰中间体结构, 目标产物收率越高|以化合物5为例, 探讨了反应温度、缚酸剂、缚酸剂浓度、反应介质等对二聚反应的影响, 确定适宜的反应条件为: 反应温度2～10 ℃, 缚酸剂选择3%～5%浓度的Na₂CO₃或KHCO₃, 反应介质为低沸点溶剂, 在此反应条件下, 化合物的收率分别为64.7%, 71.3%, 70.0%, 71.1%, 75.6%, 58.1%, 59.4%, 42.7%|利用差示扫描量热法(DSC)研究了目标化合物的热稳定性, 其中苯基取代衍生物的热稳定性较氮杂环衍生物好.     

Synthesis and characterization of NLO chromophores bearing poly(1,6-heptadiyne)s for electro-optic application

We utilized the metathesis reaction to synthesize a new type of multifunctional polymer that contains a conjugated backbone and a second-order NLO chromophore as a pendant group. The 1,6-heptadiyne derivatives bearing NLO chromophores were easily polymerized by using a metathesis catalyst to give corresponding polymers with large optical nonlinearities. Molecular structural characterizations for the resulting polymers were achieved by ¹H- and ¹³C-NMR, FTIR, and UV-visible spectroscopies. Soluble polymers were obtained up to 72 mol % of chromophore monomer portion in the copolymer. These amorphous polymers exhibited good film-forming abilities and thermal stability. The electro-optic coefficient, r₃₃, of the poled polymer films was in the range of 0.5–10.1 pm/V, and the nonresonant values of the third-order NLO coefficient, χ⁽³⁾ was found to be about 10⁻¹¹ esu. © 1996 John Wiley & Sons, Inc.     

一个新的二氮六元杂环化合物的合成、结构及表征

二氮杂环化合物及其衍生物在配合物的自组装和生物无机等领域中具有诱人的研究前景,因而引起各国化学家的广泛关注．这类化合物的合成可以追溯到60年前,Buhle等首次合成了1,5-二氮环辛烷(DACO)．随后,其一系列衍生物也被合成出来,并应用于配位化学及相关领域的研     

Synthesis and Structure Characterization of Novel Triazole Compounds Containing 1,3-Dioxolane

Five novel triazole compounds containing group 1,3-dioxolane were designed and synthesized by taking difenoconazole as the start compound and changing diphenyl ether for benzyl phenyl ether. Their structure swere confirmed by elemental analyses, ^1H NMR and IR spectra. The single crystal structure of 2-[-4-(2,4-dichlorophenylmethoxy] phenyl-2-(1,2,4-triazol-l-yl ) methane-I, 3-dioxolane was determined by means of X-ray diffraction. The preliminary bioassays showed that the synthesized compounds exhibited some activities of fungicides and plant growth regulators.     

Synthesis and Electronic Properties of Novel 5,7-Diazapentacene Derivatives

A route to the synthesis of novel 5,7-diazapentacenes and some preliminary studies on their properties is reported. A single crystal X-ray diffraction study of the dihexyl derivative showed it had formed a dimer during the analysis. The materials possess lower lying frontier orbitals than pentacene and may have potential applications in organic electronic devices. This synthetic method may be applicable to the synthesis of other azaacenes.     

1,6-亚甲基桥[10]轮烯并[3,4-g]-蒽醌衍生物的合成

采用无溶剂合成法,以1,6-亚甲基桥[10]轮烯-3,4-二甲酸酐为原料,Zr OCl2·8H2O/Na Cl为催化剂,于165℃下分别与取代苯经Friedel-Crafts缩合反应合成了4个新型的1,6-亚甲基桥[10]轮烯并[3,4-g]-蒽醌衍生物,其结构经1H NMR,13C NMR,IR,MS和HR-MS表征。