亚硝酸根的催化光度法测定

本法基于甲酸介质中，亚硝酸根对溴酸钾氧化甲基橙褪色的催化效应，用正交法确定最佳测定条件。本法测定亚硝酸根的线性范围为０～０．２０μｇ／ｍＬ灵敏度为２．８３×１０－１０ｇ／ｍＬ。用于测定水样中的亚硝酸根，结果良好。     

溴酸钾氧化吡口罗红G催化动力学光度法测定痕量NO-2

研究了在磷酸介质中亚硝酸根催化溴酸钾氧化吡口罗红Ｇ而使其褪色，建立了催化动力学光度法测定痕量亚硝酸根的新方法，测定范围为０．２～２０μｇ／ｍＬ，检出限为０．２ｎｇ／ｍＬ，用于食品和水样中的亚硝酸根测定获得满意结果     

溴酸钾氧化酸性品红催化光度法测定亚硝酸根

研究了在强酸介质中亚硝酸根催化溴钾氧化酸性品红的褪色反应及其动力学条件，建立了高灵敏测定痕量亚硝酸根的新催化光度法。方法灵敏度为３．７×１０＾－１１ｇ／ｃｍ＾２亚硝酸态氮，线性范围为０．０６－０．４２μｇ／１０ｍＬ，用于测定唾液及硝钾中亚硝酸根。     

溴酸钾氧化吡罗红G催化动力学光度法测定痕量NO2^—

研究了在磷酸介质中亚硝酸根催化溴酸钾氧化吡罗红Ｇ而使褪色，建立了催化动力学光度法测定痕量亚硝酸根的新方法，测定范围为０．２－２０μｇ／ｍＬ，检出限为０．２ｎｇ／ｍｌ，用于食品和水样中的亚硝酸根测定获得满意结果。     

动力学催化光度法测定痕量亚硝酸根

磷酸和棉红在１００℃下反应生成天蓝色物质（λｍａｘ＝６７５ｎｍ）,该物质在痕量亚硝酸根的催化下被ＫＢｒＯ３氧化褪色,研究了反应的条件,测定了动力学参数,建立了测定痕量亚硝酸根的方法,方法检出限是４＊１０＾－１０ｇ／ｍＬ,测定范围是０．４０－２０．００μｇ／Ｌ,用于水体中痕量亚硝酸根的测定,结果满意。     

高效液相色谱法同时测定血清中肌酸、尿酸和肌酐

报道了快速、简便同时测定血清中肌酸，尿酸和肌酐的ＨＰＬＣ法．以０．０２ｍｏｌ／ＬＫＨ２ＰＯ４（ｐＨ６．５）为流动相，三种物质可在２ｍｉｎ内分离，检出限分别为：肌酸０．６９μｇ／ｍＬ，尿酸０．２１μｇ／ｍＬ，肌酐０．１０μｇ／ｍＬ．     

溴连苯三酚红体系催化光度法测定亚硝酸根的研究

基于亚硝酸根以溶解氧氧化溴连苯三酚红的催经作用，建立了双波长分光光度动力学测定亚硝酸根的新方法，于３９２ｎｍ处测量体系吸光度Ａ１，４８４ｎｍ处测量体系吸光度Ａ２，以△Ａ＝Ａ１－Ａ２进行亚硝酸根定量，所建立的方法对亚硝酸根的线性范围为０．００５～１．０μｇ／ｍＬ。该法简便，灵敏，选择性好，应用于蔬菜样品的测定，结果满意。     

催化动力学光计法测定微量碘的研究

基于微量碘离子对高碘酸钠氧化甲基紫反应的催化作用，建立了测定微量碘的动力学光度法。方法检出限０．２２μｇ／ｍＬ线性范围０．３０－１．４０μｇ／ｍＬ，包括其它卤素在内的大多数阴离子、阳离子不干扰测定，用于食盐中微量碘的测定，有满意的结果。     

亚甲紫分光光度法测定微量亚硝酸根

研究了在盐酸介质中微量亚硝酸根与亚甲紫发生的重氮化反应,建立了测定微量亚硝酸根的新方法。方法的线性范围为８－４４０μｇ／Ｌ ＮＯ＾－２,检出限为８μｇ／Ｌ ＮＯ＾－２方法已用于水中微量亚硝酸根的测定,并对反应机理了初步讨论。     

亚硝酸根－对氨基苯磺酸－H酸偶联反应体系光度法测定亚硝酸根的研究

本文根据亚硝酸根与对氨基苯磺酸、Ｈ酸在酸性介质中进行的重氮偶联反应，提出了一个测定痕量亚硝酸根的分光光度新体系。最大吸收波长为５２０ｎｍ，摩尔吸光系数为３．１×１０￣４Ｌ／ｍｏｌ·ｃｍ，亚硝酸根浓度在０～１．２μｇ／ｍＬ范围内符合比耳定律．用于水样中亚硝酸根的分析，测定结果与经典的α－萘胺法一致。     

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%.     

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.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

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.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

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.     

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.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.