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1.
新西佛碱3.5—二溴水杨醛缩氨基硫脲的合成及其在荧光滴定中的应用 总被引:2,自引:0,他引:2
本文研究了新西佛碱3.5-二溴水杨醛缩氨基硫脲(简称3.5-DBSTS)的合成,及基为一种新荧光滴定指示剂,应用于有色溶液中酸碱滴定的条件,建立了一种简便,准确,快速测定有色溶液中酸碱浓度的新方法,用于有色饮料中酸含量的测定,结果满意,指示剂发光的pH突跃范围为7.48-9.72,λex=500nm。 相似文献
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5′—硝基水杨基荧光酮荧光熄灭法测定微量钨 总被引:3,自引:1,他引:3
本文基于W(Ⅵ)-5′-硝基水杨基荧光酮(5′-N-SAF)-Tween-80体系的荧光熄来效应,提出一种测定微量钨的荧光方法,在0.2~1.0mol/L的硫酸介质中,在Tween-80存在下,5′-N-SAF存在两个激发峰,其激发波分别为λex1=475nm,λex2=505nm发射波长为λem=525nm。W(Ⅵ)与5′-N-SAF形成1:3的配合物,钨浓度在每25mL0.25~2.5μg范围 相似文献
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荧光光度法测定环境水中微量甲基对硫磷 总被引:7,自引:0,他引:7
研究了荧光分光光度法测定环境水中甲基对硫磷的一。在吲哚丙酮溶液0.25%,过硼酸钠溶液0.25%溶液中,温度5℃、λex/λem=410nm/490nm,检出限5.0(5.2)μg/L,线性范围0-2.0(2.6)mg/L,回收率达98-102%,结果满意。 相似文献
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本文报道了新荧光试剂3-对甲苯基-5-(2’-羧基苯偶氨)绕丹宁(PM-PRACP)的合成。用元素分析、红外光谱、核磁共振氢谱和质谱确证了其结构,研究了其荧光性质。在pH5.6时,该试剂与Cu ̄(2+)形成稳定的荧光螯合物,且在λ_(ex)/λ_(em)=305nm/405nm产生强烈荧光。其荧光强度与Cu ̄(2+)的浓度在0~1.6μg/25mL范围内呈线性关系,检测限为5×10 ̄(-4)μg/g。已用于痕量铜(Ⅱ)的荧光分光光度法测定。测定了蚕茧、蚕丝和丝绸中的痕量铜,结果满意。 相似文献
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本文基于W(Ⅵ)-5′-硝基水杨基荧光酮(5′-N-SAF)-Tween-80体系的荧光熄灭效应,提出一种测定微量钨的新荧光方法。在0.2~1.0mol/L的硫酸介质中,在Tween-80存在下,5′-N-SAF存在两个激发峰,其激发波分别为λex1=475nm,λex2=505nm,发射波长为λem=525nm。W(Ⅵ)与5′-N-SAF形成1∶3的配合物。钨浓度在每25mL0.25~2.5μg范围内呈线性关系,检测限为每25mL0.25μg。本法灵敏度高,选择性好,不经分离可直接测定合金钢中的钨,结果满意。 相似文献
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荧光猝灭法测定微量氟的研究 总被引:1,自引:0,他引:1
建立了氟的铝-钙指示剂络合物荧光猝灭测定法。本法λex=570nm,λem=600nm,线性范围为5~160ng/mLF^-。对5ng/mlF^-重复11次测定结果的相对标准偏差为2.4%,可直接用于温泉水中氟的测定。 相似文献
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贵金属冶金物料中微量钯、铂、铑的双波长分光光度法同时测定的研究 总被引:2,自引:0,他引:2
本文提出了用二苄基二硫代乙二酰胺(DbDO)为显色剂分光光度测定铑的方法,并进一步研究了该试剂与钯、铂的反应,从而建立了可在一个试样中同时测定该三元素的方法。在2~3mol/LHC1溶液中,钯与DbDO在室温显色,用氯仿萃取并用8.4mol/LHC1振荡有机相,然后在454nm测定。在萃余液中加入SnCl_2,并在沸水浴中加热,使铂、铑的DbDO络合物生成,再用氯仿萃取,8.4mol/LHC1振荡有机相,以双波长分光光度法同时测定。其中铂用双波长系数倍率法(λ′_2=521nm,λ′_1=500nm,K=2.563),铑用双波长等吸收波长法(λ_2=400nm,λ_1=546nm)。铂和铑的含量为1:5或5:1时互不干扰。 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 相似文献
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A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL. 相似文献
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Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products. 相似文献
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A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions. 相似文献