Zur quantitativen Bestimmung von 1,5- und 2,7-Naphthalinsulfos?uren und von 2,6- und 2,7-Disulfos?uren

Ohne Zusammenfassung     

用于细胞核成像的2,7-BHVC双光子荧光探针

分别合成了2,7-双(1-羟乙基-4-乙烯基吡啶) 咔唑碘盐(2,7-BHVC)与3,6-BHVC, 进行了荧光性能和细胞核成像测试, 结果表明, 2,7位的Ф×δ是3,6位的2.8~3.6倍, 染色实验也证实了2,7-BHVC有特定成像细胞核的能力.     

新型多取代2,7-萘二甲酸二乙酯的合成

以4,6-二甲基-2-甲氧基-1,3-苯二甲酸二乙酯为原料,经Micheal加成、环化、溴化、消除等5步反应,合成新型的多取代2,7-萘二甲酸二乙酯.该合成路线步骤少,收率高,反应条件温和.产物中的4个新化合物的结构均经元素分析、核磁共振、红外光谱和质谱确证.     

2,7-TADN极谱特性研究(Ⅱ)-铜(Ⅱ)-2,7-TADN-乙二胺配合物吸附波测定痕量铜

研究了Cu²⁺-2,7-TADN-乙二胺配合物的极谱行为。在氢氧化钠、乙二胺(en)和2,7-TADN底液(pH约为12)中,铜(Ⅱ)能产生Cu²⁺-2,7-TADN-en三元配合物吸附波,其峰电位为-0.86V。铜含量在2.0×10^-8-5.0×10^-6M范围内,峰高与铜浓度成线性关系。检测下限达1.0×10^-8M。     

2,7-二甲氧基-3,6-二苯氧基萘的合成

以3,6-二溴-2,7-二羟基萘为起始原料,与硫酸二甲酯经甲醚化反应得3,6-二溴-2,7-二甲氧基萘(2);2与苯酚在碘化亚铜催化下经取代反应合成了新化合物——2,7-二甲氧基-3,6-二苯氧基萘,总收率82.5%,其结构经1H NMR,13C NMR,ESI-MS和元素分析表征。     

2,7-二芳基呫吨螺芴二醇衍生物的合成

以2,7-二溴-9-芴酮、间苯二酚和苯硼酸的衍生物为原料,经过环化、羟乙基化和Suzuki偶联等3步反应,设计并合成了一系列2,7-芳基呫吨螺芴二醇衍生物,通过红外光谱、核磁光谱(¹H NMR,¹³C NMR)、元素分析等表征了化合物的结构。折光率和紫外可见光谱测试结果表明：与2,7-无取代基的呫吨螺芴二乙醇衍生物相比,目标化合物具有更高的折光率(1.66～1.68)和良好的透光率,有望作为聚碳酸酯光学树脂的二醇单体,应用于光学透镜、光学膜等领域。     

Aggregation-Induced Emission with Large Redshift in 2,7-Diphenyl-fluorenone:Reality or Artifact?

The luminescence property of 2, 7-diphenyl-fluorenone (DPFO) was previously reported to be very unusual with a large aggregation-induced effect associated with a fluorescence redshift of 150 nm. The phenomenon is reexamined in this work. It is found that the abnormal observations are caused by the presence of a trace amount of impurity 2, 7-diphenyl-fluorene (DPF) in the as-synthesized DPFO. The pure DPFO molecule does have an intense fluorescence (FL) in solid (528 nm), about 4-5 times larger than in its dilute dichloromethane solutions (542 nm), but with a blueshifted rather than redshifted FL wavelength in solid. The enormous FL enhancement and redshifted FL wavelength of the as-synthesized DPFO solid are due to the presence of impurity DPF. The FL of DPF is much stronger than that of DPFO in dilute solutions and it also has shorter FL wavelengths. In a dilute solution of DPFO with a trace amount of DPF (~1%), the dominant FL peaks are from DPF. Because the electronic absorption peaks of DPF overlaps with DPFO, the electronic energy of DPF can transfer to DPFO. The energy transfer is faster with the increase of concentration because DPF and surrounding DPFO molecules become closer, which quenches the FL of DPF (356 and 372 nm) and enhances the FL of DPFO (542 nm in solution and 528 nm in solid). Therefore, at high concentrations or in solids, only peak at about 542 or 528 nm shows up, and peaks at 356 and 372 nm disappear.     

2,7-二溴-4-氨基芴的合成及其光学性质

以芴(1)为原料,通过溴代、硝化、还原反应合成了2,7-二溴-4-氨基芴(4),其结构经1H NMR,13C NMR,IR和ESI-MS确证。分别对溴化、硝化和还原反应条件进行优化。结果表明:在最佳溴化反应条件[CHCl3为溶剂,Cu Br2为催化剂,1 90 mmol,n(1)∶n(Cu Br2)∶n(Br2)=1.0∶0.025∶2.89,于0℃反应24 h]下,溴化产物2,7-二溴芴(2)的产率93.8%;在最佳硝化反应条件[2 30 mmol,混合酸(85%硝酸+96%硫酸)为硝化试剂,n(2)∶n(HNO3)=1.0∶4.6,于70℃反应1 h]下,硝化产物2,7-二溴-4-硝基芴(3)的产率94.7%;在最佳还原反应条件(3 30 mmol,Zn/Ca Cl2为还原剂,回流反应4 h)下,4的产率89.5%。运用UV-Vis和荧光光谱初步研究了4的光学性质。结果表明:4的λmax为352.4 nm;在352.4 nm波长激发下,4的λem位于388.4 nm和412.2 nm,光带隙低至2.66 e V。     

2,7-二硝基-9,9-二辛基芴的合成工艺改进

以芴(1)为原料,浓硝酸/浓硫酸为硝化剂,合成了2,7-二硝基-9,9-二辛基芴,其结构经1H NMR和IR确证。最佳反应条件为:1 20 mmol,n(1):n(HNO3)=1:18,c(H2SO4)=15.3 mol.L-1,于10℃反应7 h,收率56%。     

2,7-二羟基萤光黄分光光度测定微量钼(Ⅵ)

我们实验发现在阳离子表面活性剂CTMAB存在下用2,7-二羟基萤光黄分光光度测定钼不但有高的灵敏度(ε=1.33×10~5),而且与文献比较具有酸度范围宽(0.1—0.8N盐酸),显色酸度高,干扰离子相对少,试剂吸收受酸度影响小,重现性好等优点。三羟基萤光酮类是分光光度测定钼有较高灵敏度的显色剂,但受高价离子干扰严重,故必须掩蔽,尽管如此,钛、钨等的干扰仍难以消除,有用两等份试液的空白褪色法     

新显色剂2,7-二羟基萤光黄-CPB分光光度法测定微量锑

微量锑的测定,主要是采用SbCl_6~-与碱性染料孔雀绿、甲基紫等在酸性介质中缔合成三元络合物被苯、甲苯等有机溶剂萃取的分光光度法。这类方法灵敏度较高,但要用有毒的有机溶剂萃取,操作繁琐。近年来,2,3,7-三羟基-9-取代萤光酮在     

Liquid crystalline banana‐shaped monomers derived from 2,7‐naphthalene: synthesis and properties

Three banana‐shaped monomers, i.e. 2,7‐naphthalene bis[4‐(4‐allyloxyphenylazo)‐benzoate], 2,7‐naphthalene bis[4‐(4‐allyloxy‐3‐fluorophenylazo)benzoate] and 2,7‐naphthalene bis{4‐[4‐(10‐undecenyloxy)phenylazo]benzoate}, containing azobenzene as side arms, 2,7‐dihydroxynaphthalene as central units and terminal double bonds as polymerisable functional groups, were synthesised and their mesophase behaviour investigated. Polarizing optical microscopy and DSC measurements reveal that all compounds exhibit nematic mesophases. The absorption spectrum of the trans‐azobenzene groups displays a high‐intensity π–π* transition at about 365 nm and a low‐intensity n–π* transition at around 450 nm for all compounds. Hence, photochromism can be achieved by the introduction of the azo linkage to banana‐shaped liquid crystals molecules.     

高效液相色谱法测定芴酮溴代产物中2,7-二溴芴酮含量

提出了采用高效液相色谱测定芴酮溴代产物中2,7-二溴芴酮含量的方法。采用EliteHypersil ODS2 C18色谱柱(4.6 mm×250 mm,5μm)作固定相,以甲醇与水体积比为85比15的混合液为流动相,流量为1.0 mL.min-1,采用波长为254 nm的紫外检测器进行检测。2,7-二溴芴酮质量浓度在5.0~40.0 mg.L-1范围与其峰面积呈线性关系。在3个浓度水平上(即5.00,10.00,15.00 mg.L-1)对方法的回收率进行测定,测得结果在98.2%~99.1%之间,各测定值的相对标准偏差(n=6)均小于1%。     

ADSORPTIVE VOLTAMMTRIC DETERMINATION OF COPPER,NICKEL,COBALT AND CADMIUM WITH 2-QADN2,7

A new reagent 2-QADN2,7 has been synthesized and its electroana-lytical characteristics have been studied.The procedure of the adsorptivevoltammetric determination of copper,nickel,cohalt and cadmium was workedout.     

2,7-二甲基-2,4,6-辛三烯二醛的合成研究

2,7-二甲基-2,4,6-辛三烯-1,8-二醛1(2,7-dimethylocta-2,4,6-triene-1,8-dial)一直以来都被认为是合成类胡萝卜素的关键中间体之一,国外对它的合成研究起步较早,国内在2005年之前鲜有报道.     

Synthesis and Properties of Poly （aryl ether ketone） Copolymers Containing 2,7-Naphthalene Moieties

IntroductionPoly(aryl ether ketone)s are high performance en-gineering plastics with outstanding physical,chemical,thermal and mechanical properties and have been ap-plied to the aerospace industry,the electronic industry,the automobile industry,the petro…     

3,6-和2,7-咔唑衍生物单光子和双光子吸收性质的理论研究

采用密度泛函理论B3LYP方法以及ZINDO/SDCI方法计算3,6-和2,7-咔唑衍生物的分子平衡几何结构、电子结构及单光子和双光子吸收性质.乙烯基吡啶取代基的位置影响分子的单光子和双光子吸收性质.与3,6-咔唑衍生物相比,2,7-咔唑衍生物的单光子吸收波长红移,振子强度增大;双光子吸收波长红移,双光子吸收截面增加.结果表明,2,7-咔唑衍生物是更好的双光子吸收材料.