新试剂5－氟偶氮胂Ⅰ荧光法测定铝的研究

本文报道了新试剂５－氟偶氮胂Ⅰ（５－ＦＡｓＡ－Ⅰ）的合成方法，研究了荧光光度法测定铝的反应条件。Ａｌ（Ⅲ）与试剂在ｐＨ５．６０ＨＡｃ－ＮａＡｃ缓冲介质中形成１＋１红色配合物并呈现荧光，λｅｘ／λｅｍ＝３４８．６／３９１．４ｎｍ，线性范围为０～０．２μｇ／ｍＬ，检测限为３．０ｎｇ／ｍＬ。用于分析茶叶样品中的铝，结果满意。     

新试剂7-(2,4-二羟基-5-羧基苯偶氮)-8-羟基喹啉-5-磺酸与铝的荧光反应性能的研究

研究了新试剂７－（２,４－二羟基－５－羧基苯偶氮）－８－羟基喹啉－５－磺酸（简称ＤＨＣＢＡＱＳ）与铝（Ⅲ）形成的络合物的荧光性能。在ｐＨ４．６２的ＮａＡｃ－ＨＡｃ体系中形成１∶１型强荧光配合物,其λｅｘ＝５１０ｎｍ、λｅｍ＝５７２ｎｍ,铝（Ⅲ）含量在０～０．０８ｍｇ／Ｌ范围内与荧光强度呈线性关系,方法检出限为１．０４×１０－１０ｍｏｌ／Ｌ。本方法用于茶叶、淀粉及水样中痕量铝（Ⅲ）的测定。     

7—[（4—甲基2—胂酸基苯）偶氮]—8—羟基喹啉—5—磺酸荧光光度法测定氟

本文介绍了７－［（４－甲基－２－胂酸基苯）偶氮］－８－羟基喹啉－５－磺酸的合成方法以及性能，详细研究了氟对该试剂与铝形成的荧光的熄灭作用，建立了荧光法测定微量氟的新方法。应用于水样和牙膏中的氟的测定，效果良好。     

新荧光试剂DHB—8Q5S与铝的配合反应及分析应用研究

研究了新合成的试剂７－８－羟基喹啉－５磺酸荧光光度法测定铝的反应条件，铝与试剂在ＰＨ５．００－５．７５的乙酸／乙酸钠缓冲溶液中形成１＋１型配合物并呈现荧光，其最大激发波长／发射波长λｅｘ／λｅｍ＝５２２／５７０，检测下限为３×１０＾－８μｇ／ｍＬ考察了共存离子的干扰，并用于样品分析，结果满意。     

新荧光试剂DHB－8Q5S与铝（Ⅲ）的配合反应及分析应用研究

研究了新合成的试剂７－（２，４－二羟基苯偶氮）－８－羟基喹啉－５－磺酸（简称ＤＨＢ─８Ｑ５Ｓ）荧光光度法测定铝（Ⅲ）的反应条件，铝（Ⅲ）与试剂在ｐＨ５．００～５．７５的乙酸／乙酸钠缓冲溶液中形成１＋１型配合物并呈现荧光，其最大激发波长／发射波长λ_（ｅｘ）／λ_（ｅｍ）＝５２２／５７０（ｎｍ），检测下限为３×１０~（－８）μｇ／ｍＬ，考察了共存离子的干扰，并用于样品分析，结果满意。     

9-(3，5-二溴)水杨基荧光酮-溴化十六烷基三甲铵荧光光度法测定微量铝

研究了９－（３,５－二溴）水杨基荧光酮与铝（Ⅲ）的反应条件。在ＰＨ５．５的（ＣＨ２）６Ｎ４－ＨＣＬ缓冲溶液中,ＡＩ（Ⅲ）与试睡成络合物使试剂的荧光猝灭。建立了铝－９－（３,５－二溴）,水杨基荧光酮体系测定痕量铝的荧光光度法。荧光强度与铝的含量在０～１．４μｇ／ｍＬ范围内呈线性关系。本法已用于合金风标样中铝的测定。     

用新试剂2-[(5’-氟-2’-砷酸基苯)偶氮]-1,8-二羟基-3,6-萘二磺酸荧光法测定硼

研究了试剂２－［（５’－氟２’－砷酸基苯）偶氮］－１，８－二羟基－３，６－萘二磺酸与硼的荧光性能．硼与试剂形成１：２的强荧光配合物，其λｅｘ／λｅｍ＝２３４ ｎｍ／３８０ ｎｍ， Ｂ（Ⅱ）含量在 ０～３６０μｇ／Ｌ范围内呈良好线性关系，检测限为２．０６μｇ／Ｌ，据此建立了测定微量硼的新方法。该方法应用于茶叶、铝合金及粮食等样品中微量硼的测定，结果满意．     

新试剂7—（2,4—二羟基—5—羧基苯偶氮）—8—羟基喹啉—5—磺酸与铝的荧？…

研究了新试剂７－（２,４－二羟基－５－羧基苯偶氮）－８－羟基喹啉－５－磺酸形成的络合物的荧光性能。在ｐＨ４．６２的ＮａＡｃ－ＨＡｃ体系中形成１：１型强荧光配合物,其λｅｘ＝５１０ｎｍ,λｅｍ＝５７２ｎｍ,铝含量在０－０．０８ｍｇ／Ｌ范围内与荧光强度呈线性关系,方法检出限为１．０４×１０＾－１０ｍｏｌ／Ｌ。     

荧光法测定硼的研究

研究了新试剂２－［（５′－甲基－２′－胂酸茯苯）偶氮］－１，８二羟基－３，６－萘二磺到与硼的荧光性能。在ｐＨ６．７的磷酸氢二钠－磷酸二氢钾缓冲介质中，硼与试剂形成１：２的强荧光配合物，其λｅｘ／λｅｍ＝２３５ｎｍ／３６７ｎｍ，Ｂ（Ⅲ）含量在０￣２００μｇ／Ｌ范围内呈良好线性关系，检测限为０．６２９μｇ／Ｌ，建立了测定微量硼的新方法。该方法应用于茶叶及淀粉等亲品中微量硼的测定，结果满意。     

新试剂3,5—二溴—4—偶氮8—羟基喹啉苯基荧光酮光度法测定微量铝

在溴化十六烷基三甲胺（ＣＴＭＡＢ）存在下，ＰＨ６，０的ＨＡｃ－ＮａＡｃ缓冲介质中，铝与新试剂３，５－二溴－４－偶氮８－羟基喹啉苯基荧光酮形成红色三元胶束配合物，最大吸收波长位于５６４ｎｍ，表观摩尔吸光系数ε为１．３５×１０＾５．ｍｏｌ＾－１．ｃｍ＾－１，铝浓度在０～５μｇ／２５ｍＬ范围内符合比耳定律，拟定的方法用于铝铁黄铜中微量铝的测定，结果满意。     

Organoallylaluminum reagents promote easy access to trihalomethyl triazolyl homoallylic alcohols analogous to rufinamide

The results of allylation reactions employing allylaluminum reagents are described for 5-substituted (2,6-difluorobenzyl)-4-trifluoro(chloro)acetyl-1H-1,2,3-triazoles (1), in which the 5-substituents are H, Me, and Ph. The allylating reagents were generated in situ by the catalytic insertion of aluminum into allyl and crotyl bromides (2), in order to furnish a new series of twelve trihalomethyl triazolyl homoallylic alcohols (3) at yields of up to 94%. The excellent reactivity of these organoallyl reagents is highlighted as an economical alternative to the indium-mediated reactions to produce homoallylic alcohols, which are important building blocks in organic synthesis.     

Study by Methods of Electron Spin Resonance and Model Oxidation Reaction of Nanosize Metal Powders Obtained in Electric Explosion of Conductors

Paramagnetic properties of nanopowders obtained by electric explosion of copper, aluminum, cobalt, and platinum conductors have been studied. The possibility of using ESR and model reaction of isopropylbenzene for testing the electric-explosion powders as chemical reagents is discussed.     

Synthesis and characterization of highly ordered mesoporous nanomaterials Al-MCM-41 and Al-SBA-15 from bentonite as efficient catalysts for the production of biodiesel MELA and EELA

Research on Chemical Intermediates - Low-cost Al-MCM-41 and Al-SBA-15 mesoporous materials are successfully synthesized from bentonite as silicon and aluminum sources instead of laboratory reagents...     

Template-Free Synthesis of AlPO 4 -H1 by Microwave Heating

Microwave heating enhanced the crystallization of aluminophosphate gels, and AlPO 4 -H1 was successfully obtained without using organic template reagents in a short reaction time. The use of amorphous aluminum hydroxide as an aluminum source and the addition of hydrochloric acid were found to be essentially important to obtain AlPO 4 -H1 as a single phase. Nitrogen and water adsorption properties were studied by measuring the adsorption isotherms.     

A study of microporous aluminophosphates obtained in the presence of symmetrical di-n-alkylamines

Microporous aluminophosphates and silicoaluminophosphates were obtained by hydrothermal synthesis with a number of symmetrical di-n-alkylamines as templates. The influence of the reagents and chemical composition of the starting reaction gel on the phase composition of the products obtained was studied. Pure ATO-type crystals were formed when the organic component was abundant in the reaction mixture and aluminum isopropoxide served as an aluminum source. Various physicochemical investigations revealed that the properties of the products obtained depend on the amine nature.     

Evidence for a nucleophilic anti-attack on the cleaved C(2)-oxygen bond in Cl2AlH-catalyzed ring-opening of 2-substituted 1,3-dioxolanes

The Cl₂AlH-mediated ring-opening of 2-substituted cis-4-methyl-5-trifluoromethyl-1,3-dioxolanes was found to occur with regioselective cleavage of the O1-C2 bond by attack of the aluminum hydride from the direction anti to the departing oxygen. This stereochemical outcome, which appears to be unprecedented in the reductive cleavage of chiral acetals by aluminum reagents, is interpreted on the basis of theoretical calculations.     

有机铝杂环化合物的合成与应用

有机铝杂环化合物作为金属杂环化合物中的重要一员,在有机合成中表现出一些独特的性质。有机铝杂环化合物主要包括铝杂环戊二烯、铝杂环戊烯,以及铝杂环戊烷。本文介绍近年来有机铝杂环化合物的合成方法学、反应化学及其在有机合成中的应用研究进展。     

Organometallic aluminum compounds derived from 2-(1,3,5-dithiazinan-5-yl)ethanol ligands

The reactions of AlMe(2)Y (Y = Me or Cl) with new ligands 2-(1,3,5-dithiazinan-5-yl)ethanol (1), 2-(1,3,5-dithiazinan-5-yl)-1-methylethanol (2), and 2-(1,3,5-dithiazinan-5-yl)-1-phenylethanol (3) are described. The ligands are coordinated to aluminum atoms by nitrogen and oxygen atoms, with a nitrogen based spiranic structure. Equimolar reactions gave dimeric structures bearing pentacoordinated aluminum atoms O-(AlMeY)-2-(1,3,5-dithiazinan-5-yl)ethanolates (4-7) as well as monometallic compounds with tetracoordinated aluminum atoms O-(AlMeY)-2-(1,3,5-dithiazinan-5-yl)ethanolates (8-9). Reactions with 2 equiv of the aluminum reagents afforded tetracoordinated dialuminum complexes O-(AlMeY)-O-(AlMe(2)Y)-2-(1,3,5-dithiazinan-5-yl)ethanolate (10-18). The structures of the new compounds were determined by NMR ((1)H,(13)C, and (27)Al) and complemented by X-ray diffraction of compounds 4, 10, and 16-18. Relevant intermolecular interactions C-H...S, C-H...Cl, and C-H...pi found in the crystalline network are reported.     

Synthesis and purification of aluminum isopropylate

Possibility of deep purification of lower aluminum alcoholates used to synthesize aluminum oxide by the sol-gel method and pyrolytic technique is analyzed. The influence exerted by the purity of the starting reagents, moisture content, and catalyst on the nature of the process and the purity of the product being obtained was examined.     

Copper-catalyzed desymmetrization of oxabenzonorbornadienes with aluminum reagents

The desymmetrization of oxabenzonorbornadienes with aluminum reagents and SimplePhos as chiral ligand is described. The corresponding homoallylic alcohols are obtained in high yield, diastereoselectivity, and enantiomeric excess. Furthermore the first anti enantioselective desymmetrization with aromatic nucleophiles is reported.