催化动力学光度法测定芦丁

在氢氧化钠介质中,芦丁对高碘酸钾氧化偶氮胂Ⅲ褪色反应有明显的催化作用,据此建立了测定芦丁含量的催化动力学光度法.最大吸收波长为590nm,该方法的线性范围为0.03～1.0mg/L.对实验数据进行回归处理的线性方程为ΔΑ=0.4485c(芦丁)+0.0011,相关系数为r=0.9985,检出限为0.0167mg/L.该方法简便,快速,灵敏度高,用于实际样品的测定,结果令人满意.     

阻抑催化褪色光度法测定痕量绿原酸

在盐酸介质中 ,绿原酸能灵敏地阻抑铁 催化过氧化氢还原亮绿SF的褪色指示反应 ,据此建立了测定痕量绿原酸的阻抑 催化动力学光度分析方法。该方法测定绿原酸的线性范围为 0～ 0 .12mg/L ;检出限为4 .2× 10 -6g/L。对浓度为 0 .0 8mg/L绿原酸标准溶液 6次平行测定的相对标准偏差为 3.8% ;回收率为 93.4 %～ 10 5 %。考察了反应的最佳条件和动力学参数 ,探讨了反应机理。该方法应用于金银花浸取液中绿原酸含量的测定 ,结果满意     

动力学光度法测定芦丁的研究

在氢氧化钠介质中,微量芦丁对高碘酸钾氧化罗丹明6G褪色反应有明显的催化作用,据此建立了测定芦丁含量的动力学光度分析法。方法的线性范围为0.02～1.5μg/mL,检出限为1.0×10-8g/mL。测定了反应动力学参数。方法用于芦丁片剂中芦丁含量的测定,结果令人满意。     

毛细管电泳法测定复方芦丁片中的芦丁和维生素C

用毛细管电泳紫外检测法同时测定了复方芦丁片中芦丁和抗坏血酸的含量 ,研究了各种条件的影响 ,得到了优化的实验条件 ,在 30 mmol/L Na2 B4 O7-H3BO3( p H7.5 0 )缓冲溶液中 ,芦丁和维生素 C在 1 3min内得到了良好的分离 ,芦丁和维生素 C分别在 0 .5～ 0 .0 0 5 mg和 5 .0～ 0 .0 5 mg浓度范围内与电泳峰高呈现良好线性关系 ,检测下限分别为 0 .0 0 2 mg和 0 .0 1 mg,应用于实际样品的测定     

氧化酸性铬蓝K褪色动力学光度法测定微量芦丁

基于2 mmol/L的H2SO4介质中,微量芦丁催化H2O2氧化酸性铬蓝K(ACBK)的褪色反应,建立了测定微量芦丁的动力学光度法。方法的检出限为1.08μg/L,线性范围为3.6~400μg/L。实验讨论了酸度、反应物浓度、温度、反应时间、干扰离子等因素的影响,确定了该体系反应的最佳条件,并测定了一些动力学参数,催化反应的表观活化能为73.22 kJ/mol。在25 mL溶液中,测定10.0μg芦丁的相对标准偏差为1.6%(n=11)。方法用于测定槐米和芦丁片剂中的芦丁,相对标准偏差为1.0%~1.1%,标准加入回收率为98.0%~101.7%。     

痕量铁催化对氨基二甲替苯胺-H酸显色反应

研究了在pH =5 .7混合酸 氢氧化钠缓冲介质中 ,铁 催化过氧化氢氧化对 氨基二甲替苯胺盐酸盐和H酸 钠盐的氧化偶联反应 ,考察了反应的最佳条件 ,建立了催化动力学光度法测定痕量铁 的新方法。该方法线性范围为 0 .0 0～ 0 .0 2mg L ;检出限为 2 .1× 1 0 - 7g L。直接用于自来水及湖水中铁 的测定 ,结果满意     

阻抑动力学光度法测定微量间苯二酚

基于硫酸介质中 ,间苯二酚对 Fe( )催化 H2 O2 与罗丹明 B之间褪色反应的抑制作用 ,建立了一种测定微量间苯二酚的新方法 ,并研究了反应的最佳条件和动力学参数。该方法测定的线性范围为 0 .2 0～ 3.0 mg/L,ε564 =1 .3× 1 0 4L· mol-1· cm-1。可用于水样中间苯二酚的测定     

阻抑动力学光度法测定废水中的痕量对苯二胺

在硫酸介质中,对苯二胺能灵敏地阻抑Cu（Ⅱ）催化高碘酸钾氧化孔雀绿的褪色反应。研究了该阻抑褪色反应的最佳条件,并据此建立了测定痕量对苯二胺的阻抑催化动力学光度分析方法,对苯二胺的线性范围为0．6～4．0mg／L,检出限为0．33mg／L。将该方法应用于模拟废水中对苯二胺含量的测定,测定结果的相对标准偏差为2．1％～2,3％,对苯二胺的加标回收率为99％-103％。     

新体系催化动力学光度法测定痕量亚硝酸根

基于增敏剂吐温 - 80存在下亚硝酸根催化过氧化氢氧化中性红的反应 ,建立了测定痕量亚硝酸根的新催化动力学光度法。方法的灵敏度较常规方法提高了 2 .2倍 ,测定的线性范围为 2～ 1 0 μg/L,检出限为 2 .7× 1 0 - 10 g/m L。已用于测定水样中 NO2 - 的含量     

动力学光度法测定痕量邻菲咯啉

在稀醋酸介质中,痕量邻菲咯啉对高碘酸钾氧化玫瑰桃红R褪色反应有明显的催化作用,据此建立了测定邻菲咯啉的催化动力学光度法。讨论了反应的动力学参数。方法的线性范围为0．005—0．1mg／L;检出限为3.0μg／L。方法灵敏度高,简便,快速,选择性好,用于合成水样及废水、河水中邻菲咯啉含量的测定,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%.     

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.     

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.     

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.     

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.     

Microwave-assisted copper-catalyzed stereoselective ring expansion of three-membered heterocycles with α-diazo-β-dicarbonyl compounds

Microwave-assisted copper-catalyzed ring expansions of three-membered heterocycles with α-diazo-β-dicarbonyl compounds were investigated. Thiiranes generated 3-acyl-5,6-dihydro-1,4-oxathiines in the presence of copper sulfate and trans-3-acyl-5,6-dihydro-1,4-oxathiines as stereospecific products for 1,2-disubstituted cis-thiiranes through an intramolecular S_N2 process. Oxiranes gave rise to 2-acyl-5,6-dihydro-1,4-dioxines under the catalysis of copper hexafluoroacetylacetonate and cis-3-acyl-5,6-dihydro-1,4-dioxines as stereospecific products for 1,2-disubstituted cis-oxiranes via an intimate ion-pair mechanism. The current method provides a direct and simple strategy in efficient preparation of 3-acyl-5,6-dihydro-1,4-oxathiines and 2-acyl-5,6-dihydro-1,4-dioxines, important agents in medicinal and agricultural chemistry, from readily available thiiranes and oxiranes, respectively.     

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.     

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%).