2-[2′-苯并噻唑偶氮]-1,8-二羟基萘-3,6-二磺酸的合成及与铝的显色反应研究

本文合成了新的显色试剂2-〔2’-苯并噻唑偶氮〕-1,8-二羟基萘-3,6-二磺酸,并研究了与铝的显色反应.在CTMAB存在下,铝与试剂于pH7.0～8.0的缓冲溶液中形成稳定的深紫红色络合物,组成为Al(Ⅱ):R=1:2表观摩尔吸光系数为1.46×10~5L·mol_(-1)·cm~(-1).铝浓度在0～5.0 μg/25mL范围内符合比尔定律.该方法灵敏度高,选择性好,并用于测定低合金钢、稀土硅镁合金和硅铁等试样中的微量铝.     

铝与络黑T显色反应的研究和应用

研究了络黑T(EBT)与铝发生显色反应的适宜条件。在0.15mol·L-1NaOAc溶液中,发生配位反应生成紫色的二元配合物,配位比为Al∶EBT=1∶3。最大吸收波长为536nm,ε值为1.9×104L·mol-1·cm-1,线性范围为0～30μg/50ml。方法可用于一些胃药中铝的测定,测定结果与络天青S法十分吻合。     

分光光度法测定碳酸钠及水样中的痕量铝

铝是人体必需微量元素之一 ,但含量过高有害于健康。本文研究了铝 (Ⅲ )与DBC 偶氮氯膦(DBC CPA) [1 ] 显色反应 ,在pH4 7HAc NaAc缓冲体系中 ,该试剂可与Al(Ⅲ )形成 1∶1紫蓝色络合物 ,最大吸收波长为 62 0nm ,ε62 0nm=1 38× 1 0 4 L·mol- 1 ·cm- 1 ,铝 (Ⅲ )在 0～ 35 μg/2 5mL范围内遵守比耳定律。本法用于雨水及碳酸钠中痕量铝的测定 ,结果满意。1　实验部分1 1　主要试剂铝标准溶液 :准确称取 1 75 82gKAl(SO4) 2 ·1 2H2 O ,溶于水后定容至 1 0 0mL ,得铝 1 0 0 0mg·mL- 1 储备液 ,移取适量储备液稀释后得铝 1 0…     

对乙酰基偶氮胂吸光光度法测定微量铜

在pH5.0的(CH2)6N4-HCl缓冲介质中,Cu(Ⅱ)与对乙酰基偶氮胂(ASApA)形成1比2络合物,λmax＝598nm,εmax=1.30×104L·mol-l·cm-1,铜浓度在0～2.0mg·L-1范围内遵从比耳定律。方法用于粮食、食品、水、树叶及人发等试样中铜的测定,结果满意。     

《理化检验》化学分册第30卷(1994年)总目次

研究与试验招告用页翔页某些安替比林偶氦苯甲醛类试剂与钮l显色dg研（la（回）-5-Br-PADAP-TrltonX-100析相光度法测计……………………………………………………17定矿石中微量惊……………··、·、…………………·124流动注的-火焰原子吸收光度法剑定烧碱中铁液膜富集与人焰原子吸收光谱测定饮料中痕量锌…··、………………………………………………··19………………………………………………·、··、…·1266-取代苯并喳陛偶氮苯甲酿型试剂与铁铂镍用钮流动注射氢比物石垦炉原子吸收法测定铝锑合金显色的反阿—………………     

新试剂1-(2,6-二溴-4-硝基苯)-3-(4-硝基苯)-三氮烯与汞的显色反应及应用

三氮烯试剂与第ＩＢ、ＩＩＢ族金属元素有高灵敏的显色反应 1 [1] ,可用来测定样品中微量的Ｃｄ2 + 、Ｈｇ2 + 、Ｚｎ2 + 、Ｎｉ2 + 。随着表面活性剂引入该显色体系 ,使该试剂与金属离子显色反应的灵敏度有了很大的提高。目前报道的三氮烯显色剂与Ｈｇ2 + 显色反应的灵敏度一般在ε =1 .0× 1 0 5Ｌ·ｍｏｌ-1·ｃｍ-1左右 ,但也有部分试剂的灵敏度较高 ,如ＯＣ Ｃａｄｉｏｎ[2 ] 的ε =1 .77× 1 0 5Ｌ·ｍｏｌ-1·ｃｍ-1,ＤＮＡＡＢ[3 ] ε=1 .74× 1 0 5Ｌ·ｍｏｌ-1·ｃｍ-1,ＭＤＡＡ[4]的ε=1 .8× 1 0 5Ｌ·ｍｏｌ-1·ｃｍ-1,ＡＰＤ…     

贵金属高灵敏显色反应的研究(Ⅰ) 金(Ⅲ)-碘化钾-丁基罗丹明B-明胶体系

贵金属已知的显色反应中,除萃取浮选的以外,摩尔吸光系数(ε)达到或超过2×10~5I·mol~(-1)·cm~(-1)者为数甚少。就金来说,目前以乙基硫代米嗤酮的灵敏度最高(ε=1.95×10~5l·mol~(-1)·cm~(-1)),甲基硫代米嗤酮次之(ε=1.6×10~5l·mol~(-1)·cm~(-1))。碱性染料如罗丹明B与AuCl_4~-缔合萃取显色反应ε=9.7×10~4l·mol~(-1)·cm~(-1)。有关金(Ⅲ)-碘化钾-碱性染料体系显色反应仍未见报道。我们发现在明胶、TritonX-100和抗坏血酸存在下Au(Ⅲ)与KI、罗丹明B特别是丁基罗丹明B的显色反应具有很高的灵敏度,有色络合物的摩尔吸光系数分别为2.3×10~5l.mol~(-1)·cm~(-1)(罗丹明B)和1.2×10~6l·mol~(-1)·cm~(-1)(丁基罗丹明B),特别是后者,ε值之高实属罕见,故我们称之为超高灵敏显色反应。     

分光光度法则定航空润滑油中微量铝

本文在文［１－４］的基础上，研究了在溴化十六烷基三甲基铵（ＣＴＭＡＢ）存在下铝与水杨基萤光酮（ＳＡＦ）的显色反应。在ｐＨ４．９的介质中，配合物的最大吸收峰位于５５２ｎｍ，表观摩尔吸光系数为１．１４ｘ１０￣５Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１）。铝与水杨基萤光酮的络合比为１：２。铝量在０－７．０μｇ／２５ｍｌ范围内符合比耳定律。该体系是光度法测定铝的灵敏显色反应之一，方法有一定选择性，用于航空润滑油中铝的测定，结果较为满意。     

Al-CAS-TPB-乙醇四元显色体系光度法测定微量铝

光度法测铝目前主要为三元显色体系。我们在前人工作的基础上,研究了Al-铬天菁S(CAS)-溴化十四烷基吡啶(TPB)-乙醇四元显色体系的显色条件。实验表明在pH4.6—6.0范围内络合物吸光度最大且恒定不变,络合物最大吸收波长为650nm(未校正波长),摩尔吸光系数为1.5×10~5cm~(-1)·mol~(-1)。     

3,5—二溴—4—氨基苯基荧光酮与铝显色反应的研究及应用

研究了在阳离子表面活性剂CTMAB存在下,铝与3,5-二溴-4-氨基苯基荧光酮形成配合物的显色反应。在pH 6.5的乙酸-乙酸钠缓冲溶液中Al(Ⅲ)-DBAPF-CTMAB配合物最大吸收峰位于559nm波长处,表观摩尔吸光系数为1.25×10~5,铝含量在0～0.19μg·ml~(-1)范围内服从比耳定律。拟定方法用于铝铁黄铜及石灰石样品中微量铝的测定,结果满意。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

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%.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

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.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

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.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

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.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

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.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

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.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

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.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

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.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.