一种水溶性1,8-萘酰亚胺荧光化合物的合成及性能研究

以N,N-二甲氨基丙胺和4-溴-1,8-萘酸酐为原料,吡啶为溶剂,一步法合成了一种水溶性的1,8-萘酰亚胺荧光分子,4-(N,N-二甲氨基丙氨基)-N-(N,N-二甲氨基丙基)-1,8-萘酰亚胺,以1H NMR和质谱对产物的结构进行表征,考察了浓度、pH和溶剂对该化合物荧光性能的影响。     

含噻二唑杂环的1,8-萘酰亚胺衍生物的合成与表征

以4-溴-1,8-萘酐为起始原料,通过硝化、亲电取代、氢化还原、关环和亚酰化反应,合成了目标产物3,4-[1,2,3]-噻二唑-N-丙基-1,8-萘酰亚胺和3,4-[1,2,3]-噻二唑-N-丁基-1,8-萘酰亚胺.     

1,8-萘酐类水溶性荧光染料的合成

通过在1,8 萘酐4 位的烷基链上形成季铵盐亲水基团,合成了两个以1,8 萘酐为母体的水溶性荧光染料。以4 Br 1,8 萘酐为原料,经胺化、酰胺化、季铵盐化3步反应,合成了季铵盐型4 (N′,N′ 二甲基 1 哌嗪基) N 烷基 1,8 萘酰亚胺,总收率达到70 2%以上。目标化合物在水溶液中的量子收率达到0 6以上。     

维生素B1催化合成2-乙基-2-甲基-2,3-二氢-1H伯啶

研究了在维生素B1催化下,以无水乙醇为溶剂,1,8-二氨基萘与丁酮反应合成2-乙基-2-甲基-2,3-二氢-1H伯啶的反应,考察了催化剂用量、反应物摩尔比、反应温度、时间等因素对产品收率的影响。结果表明,在电磁搅拌下,当1,8-二氨基萘用量为0.1 mol,丁酮与1,8-二氨基萘的摩尔比在1.2∶1,催化剂用量为2.0%,反应温度为35℃,反应30 min时,最佳产品收率可达到85.2%。维生素B1对该反应具有良好的催化作用,是合成2-乙基-2-甲基-2,3-二氢-1H伯啶的良好催化剂。产品经熔点、红外光谱进行了表征。     

基于1,8-萘酰亚胺功能团的Hg2+荧光分子探针的合成与性能

以4-溴-1,8-萘酐和正丁胺为原料,合成了含有l,8-萘酰亚胺官能团的汞离子荧光分子探针4-二(2-羟乙基氨基)-乙氨基-N-n-丁基-1,8-萘酰亚胺(FP).采用红外光谱、质谱及核磁共振氢谱等测试技术对产物进行了结构表征.考察了Cd2+、Hg2+、Na+、pb2+、Co2+、Mg2+、Ca2+、Fe3+、Cu2+...     

8-碘-1-萘甲醛的合成

以1,8-萘二酸酐为起始原料,经过汞代脱羧、碘代、甲酯化、还原和氧化等5步反应合成标题化合物。原料易得,操作简单,反应条件温和,总收率达48%。     

萘-1,4-二腈合成新工艺

本文介绍了一种合成萘-1,4-二腈的新路线,该路线按生产要求对工艺条件进行了优化。邻二氯苄经过腈化与N,N′-二异丙基-二亚氨基乙烷缩合制备萘-1,4-二腈,总收率73%,纯度99.5%。标题化合物结构经过鉴定得到确认。     

2-(3-(二甲氨基)丙基)-6-((2-硝基苯基)氨基)-1H-苯并[de]异喹啉-1,3(2H)-二酮的合成

先以4-溴-1,8-萘酐和二甲基氨基丙胺为原料经酰化反应合成中间体,再与邻硝基苯胺进行Buchwald-Hartwig偶联反应得到目标化合物。     

1,8-萘酰亚胺接枝聚磷腈合成工艺研究

研究了以4-溴-1,8-萘酐与聚二氯磷腈为原料合成具有荧光性的高分子材料4-乙氧基-N-羟乙基-1,8-萘酰亚胺接枝聚氯磷腈的合成工艺,并用紫外光谱和傅立叶红外光谱(FT-IR)对合成产物进行了表征。     

2,2-二甲基-2,3-二氢(口白)啶的合成

以1,8-二氨基萘和丙酮为原料,无水乙醇为溶剂,对甲苯磺酸催化下合成了2,2-二甲基-2,3-二氢（口白）啶。适宜的反应条件为:原料摩尔比（1,8-二氨基萘/丙酮）1:1.5,对甲苯磺酸用量 1％（以1,8-二氨基萘计）,反应时间1.0小时,反应温度为55～60℃,收率为84.0％。UV、IR、HMR符合结构特征。滤液循环套用后,产品收率由84.0％提高到92.9％;套用4次时,产品质量基本稳定。     

4-丁胺-N-氨基吡啶-1,8-萘酰亚胺的合成及金属离子识别作用研究

以4-溴-1,8-萘酐为起始原料,通过与N-氨基吡啶发生酰化反应制得4-溴-N-氨基吡啶-1,8-萘酰亚胺后,再与正丁胺缩合得到目标化合物,并以荧光光谱法研究了目标化合物对Cd^2+、Cr^3+、Cu^2+、Fe^3+、Sm^3+、K^+、La^3+、Mg^2+、Ba^2+、Zn^2+、Ni^2+、Ir^3+、Al^3+13种金属离子的识别作用。结果表明,随着各种金属离子的加入,目标化合物的荧光光谱发生了不同程度猝灭现象;在pH 7.40时,目标化合物对Fe^3+的识别作用最优,检出限为2.55×10^-3 mol/L,配合常数为6.02×10^5 L/mol,表现出良好的选择性。     

亨克尔反应制备2,6-萘二甲酸

以1,8-萘二酸酐为原料与氢氧化钾溶液反应制备1,8-萘二甲酸二钾盐,后在萘为传热介质下异构化合成2,6-萘二甲酸。通过高效液相色谱分析产物,确定反应的收率以及酸值;用核磁、质谱和红外光谱鉴定反应产物,并探讨了催化剂选择与浓度、萘的用量、反应温度、反应时间等对亨克尔反应的影响。结果表明:虽然碘化锌催化剂的催化效果比碳酸锌好,但其在反应过程中会转化为碳酸锌;在萘添加量为反应原料的3倍,碳酸锌摩尔分数为10%,碘化钾摩尔分数为20%,反应温度450℃,反应时间90 min条件下,2,6-萘二甲酸的收率可以达到44.1%。     

2,6-萘二甲酸的合成研究

使用1,8-萘二甲酸酐为原料,采用亨克尔法,以碳酸锌做催化剂、萘和碘化钾为助剂,在二氧化碳气氛中进行反应,通过异构化反应制备2,6-萘二甲酸.探讨了反应温度、反应时间、催化剂用量、反应压力、搅拌速度、助催化剂和助剂用量对异构化转位反应的影响.结果表明:根据正交实验确定了1,8-萘二甲酸二钾盐异构化转位反应的较优工艺,各...     

Effect of comonomers on the rate of crystallization of PET: U‐turn comonomers

The effect of incorporating phthalate, 1,8‐naphthalenedicarboxylate, and 1,8‐anthracenedicarboxylate structural units on the crystallization rate of PET are evaluated by isothermal and dynamic calorimetry. Although all of the comonomers retard crystallization, the 1,8‐naphthalene unit shows no concentration dependence between 2.5 and 10% incorporation, in contrast to the smaller phthalate and larger anthracene units. The greater rate at which the 1,8‐naphthalene copolymer crystallizes, relative to that of the other copolymers, is consistent with the notion that the U‐turn geometry induces chain folding and nucleates crystallization. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 1675–1682, 2001     

Brominated Diamino Dihydroxyanthraquinones. Blue Dyes for Synthetic-polymer Fibres

The synthesis of all the isomeric mono-, di-, tri and tetrabromo derivatives of 1,8-diamino-4,5-dihydroxyanthraquinone and of 1,5-diamino-4,8-dihydroxyanthra-quinones is described. The effect of the number and orientation of bromine atoms on the dyeing and fastness properties of these dyes on polyester fibres is reported. Synergistic effects pertinent to the dyeing and fastness properties of mixtures of unbrominated and brominated derivatives are also noted.     

The Synthesis and Characterization of Melamine Based and [Fe/CrSalen] or [Fe/CrSalophen] Capped Polimer Schiff Base Complexes

In this study, by using previously reported monomer complexes [(2-(4-carboxybenzimino)-4,6-diamino-1,3,5-triazine)(salen/salophenFeIII)], [(2-(4-carboxybenzimino)-4,6-diamino-1,3,5-triazine)(salen/salophenCrIII)], [(2-(3,4-dihydroxybenzimino)-4,6-diamino-1,3,5-triazine)(salen/salophenFeIII)] and [(2-(3,4-dihydroxybenzimino)-4,6-diamino-1,3,5-triazine)(salen/salophenCrIII)] obtained by Uysal and Uçan (J Inc Phenom Macrocycl Chem, in press), sixteen new polimer Fe(III) and Cr(III) complexes involving tetradentate Schiff bases N,N′-bis (salicylidene)ethylenediamine-(salenH₂) or bis(salicylidene)-o-phenylenediamine-(salophenH₂) with 2-(4-carboxybenzimino)-4,6-diamino-1,3,5-triazine or 2-(3,4-dihydroxybenzimino)-4,6-diamino-1,3,5-triazine (Uysal and Uçan, J Inc Phenom Macrocycl Chem, in press) and terephthaldehyde or glutaraldehyde have been synthesized and characterized by means of elemental analysis, ¹H N.M.R., FT-IR spectrscopy, MS, thermal analyses and magnetic susceptibility measurements. The complexes have also been characterized as low-spin distorted octahedral Fe(III) and Cr(III) bridged by catechol and/or COO^? groups.     

聚丙烯催化剂内给电子体二乙酸-1,8-萘酚酯的合成与表征

以1,8-萘二酚和乙酰氯为原料,以三乙胺为吸收剂合成了二乙酸-1,8-萘酚酯,采用了红外光谱和核磁共振氢谱等分析测试手段对产品进行了结构表征并逐一归属。考察了原料配比、反应时间、反应温度及吸收剂用量等因素对二乙酸-1,8-萘酚酯收率的影响。实验结果表明,合成二乙酸-1,8-萘酚酯的最佳工艺条件为:1,8-萘二酚0.1 mol,n(1,8-萘二酚)︰n(乙酰氯)=1.0︰2.4,三乙胺吸收剂为60 mL,反应温度25℃,反应时间5.0 h,在此条件下,二乙酸-1,8-萘酚酯收率可达88.4%。     

Structural and Optical Properties of New Naphthalene and Perylene Imide Imidazoles

ABSTRACT

New unsymmetrically substituted naphthalene and perylene imide imidazoles, N-(2-ethylhexyl)-naphthalene-3,4-(4,5-dicyano-1,2-benzimidazole)-9,10-dicarboxyimide and N-(1-heptyloctyl)-perilene-3,4-(4,5-dicyano-1,2-benzimid-azole)-9,10-dicarboxyimide, were synthesized via condensation reactions of diaminophthalonitrile and aromatic monoimide monoanhydride derivatives. Their structural analyses have been conducted by using general spectroscopic methods including FT-IR, ¹H- and ¹³C-NMR, mass and elemental analysis. The molecular structure of naphthalene derivative was also determined by single crystal x-ray diffraction. Electronic absorption and emission properties were investigated on comparison. For studied compounds, both DFT and TDDFT calculations were carried out with the 6-311G(d,p) basis set, taking into account solvation effects by means of polarizable continuum model as implemented in the Gaussian 09 package.     

Molecular dynamics study on thermal and mechanical properties of AOO modified DGEBA-anhydride insulating materials for high voltage GIS

Increases in rated voltage and power density of high voltage gas insulated switchgears (GIS) impose stringent requirements on the diglycidyl ether of bisphenol A (DGEBA)-anhydride thermoset, which is widely used as insulation materials for high GIS, for higher mechanical and heat-resistant properties. In this paper, 3,4-epoxycyclohexylmethyl 3,4-epoxycyclohexanecarboxylate (AOO) was copolymerized with DGEBA -anhydride system to increase the mechanical and thermal properties of the thermosets. Based on the molecular dynamics simulation method, the coefficient of thermal expansion, glass transition temperature (T_g), and modulus of AOO copolymer-modified DGEBA-anhydride thermosets were calculated. The AOO copolymer-modified DGEBA-anhydride thermosets specimens were further experimentally prepared and subjected to differential scanning calorimeter test, TGA test, tensile bending test, and dielectric test. The results of simulation and experiment simultaneously indicated that the T_g and modulus of the DGEBA-anhydride thermoset are enhanced after AOO modification. This is mainly due to the decrease in free volume percentage and mean square displacement of the epoxy cross-linked network structure after the introduction of AOO molecules, which makes the structure more compact and the cross-link density increased. Additionally, the dielectric performances of the thermoset was enhanced by AOO. The excellent thermal, mechanical and dielectric properties of AOO modified DGEBA-anhydride thermoset make it a promising application in the field of high voltage GIS.     

维生素B1催化合成2，2-二甲基-2，3-二氢伯啶

研究了在维生素B1催化下,以无水乙醇为溶剂,1,8-二氨基萘与丙酮反应合成2,2-二甲基-2,3-二氢伯啶的反应,考察了反应温度、搅拌时间、催化剂用量、反应物摩尔比等因素对产品收率的影响。结果表明,在电磁搅拌下,当1,8-二氨基萘用量为0．1mol,1,8-二氨基萘与丙酮的摩尔比为1：1．2,催化剂用量为1．2％,反应20min,反应温度为30℃时,维生素B1对该反应具有良好的催化作用,产品收率可达到93．6％。产品经熔点、红外光谱进行了表征。