溴邻苯三酚红褪色光度法测定食盐中碘的研究

在硫酸介质中,碘酸根能氧化溴邻苯三酚红使之褪色,且褪色的程度与碘酸根的存在量有关,从而建立了光度法测定碘的方法。有色溶液的最大吸收波长为510nm,碘的存在量在0～30μg/25ml范围内符合比耳定律,表观摩尔吸光系数ε=1.81×104L·mol-1·cm-1。方法简便、快速、选择性好,准确度高,用于测定食盐中微量碘时,结果满意。     

甲基红氧化褪色光度法测定食盐中碘

基于在盐酸介质中 ,碘酸根在溴化钾的催化作用下使甲基红氧化褪色的反应 ,建立了测定微量碘的新方法。方法的线性范围为 8μg/2 5mL～ 2 2 μg/2 5mL ,表观摩尔吸收系数为 6 .5× 1 0 4 L·mol- 1 ·cm- 1 ,已用于食盐中碘的测定。     

二甲基黄褪色光度法测定微量碘

在硫酸介质中,溴化钾催化下,碘酸根对二甲基黄有褪色作用,且褪色的程度与碘酸根的量有关,从而建立了光度法测定碘的新方法。方法的最大吸收波长为515nm,表观摩尔吸光系数为3.1×104L·mol-1·cm-1,碘浓度在0～20μg/10ml范围内符合比耳定律,检出限为1.02×10-8g·ml-1。方法简单、快速、选择性好、灵敏度高,用于测定碘盐中碘的含量,结果满意。     

钙羧酸钠褪色光度法测定微量碘的研究

提出了以钙羧酸钠褪色光度法测定微量碘的新方法。在盐酸介质中 ,表面活性剂十六烷基三甲基溴化铵 (CTMAB)存在下 ,碘酸根离子定量氧化钙羧酸钠褪色。最大吸收波长λmax=5 95nm ,表观摩尔吸光系数ε =3.1× 10 4 L·mol-1·cm-1。碘浓度在 0～ 5 0 μg 2 5ml范围内服从比耳定律。方法用于加碘食盐中碘的测定 ,结果满意     

二甲酚橙褪色光度法测定微量碘的研究

研究了在硫酸介质中,溴化钾催化下,碘酸根氧化二甲酚橙褪色的最佳条件。其最大吸收波长λmax为430nm,表观摩尔吸光系数为1．3×104L·mol-1·cm-1,碘浓度在0-30μg／25ml范围内呈线性关系。方法用于测定加碘食盐中碘,回收率可达98．0％-101．3％,结果满意。     

甲基红褪色光度法测定食盐中碘的研究

在酸性介质中,溴化钾存在下,碘酸根对甲基红有褪色作用,且褪色的程度与碘酸根的量有关,从而建立了碘的光度测定新方法。方法的最大吸收在520nm处,碘定量测定的线性范围为0～16μg/10mL,检出限为1.47×10-8g/mL。方法操作简单、快速、重现性好,用于加碘食盐中碘的测定,结果满意。     

中性红氧化褪色光度法测定海带中的微量碘

讨论了用H2SO4-KBr-IO3--中性红氧化褪色光度法测定海带中微量碘的方法。在酸性介质中,以KBr作为催化剂,碘酸根对中性红有褪色作用,且褪色的程度与碘酸根的量有关,碘定量测定的线性范围为0~25μg/mL,表观摩尔吸收系数ε=1.79×104L.mol-1.cm-1。回收率97.1%~101.7%。该法是测定海带中微量碘的一种较理想的方法。     

甲基橙氧化褪色吸光光度法测定碘的研究

提出了在硫酸介质中并在溴化钾的催化下,碘酸根氧化甲基橙褪色吸光光度法测定碘的新方法.试验结果表明,在最大吸收波长510nm处,碘浓度在0～50μg/50ml范围内呈线性关系,表观摩尔吸光系数为9.0×10~(4).方法已用于测定碘盐及海带中的碘,结果满意.     

酸性红褪色分光光度法测定食盐中碘的含量

研究了在H_2SO_4-KBr的介质中,碘酸钾能够氧化酸性红并使之褪色,且褪色的程度与碘酸根的含量在一定范围内有很好的线性关系,从而建立了一种新的测定碘的方法。实验结果表明,酸性红的最大吸收波长为510nm,碘的含量在0～50μg/50mL范围内,符合比耳定律,其回归方程为△A=0.004 13C+0.032 14,相关系数R2=0.998 3,检出限为0.78μg/50mL。方法操作简单,快速准确,用于食盐中碘含量的测定,结果令人满意。     

碘酸根与3,3‘,5,5’—四甲基联苯胺的显色反应研究及其分析应用

研究了碘酸根与 3,3′,5 ,5′-四甲基联苯胺 (TMB)的显色反应 ,建立了测定微量碘的分光光度法。在盐酸介质中 ,碘酸根能定量氧化 TMB生成黄色的TMB亚胺盐 ,其最大吸收波长为 45 0 nm,表观摩尔吸光系数为 2 .13× 10 5 L·mo1-1·cm-1 ,碘的质量浓度在 0～ 0 .7mg/ L 范围内符合比尔定律 ,该法已应用于加碘酸钾食盐中碘含量的测定     

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.