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.     

气浮溶剂浮选光度法测定食品中痕量SO32-的研究

提出了碘溴化十六烷基三甲胺缔合体系溶剂浮选褪色光度法测定SO2-3 的新方法,方法的摩尔吸光系数ε365=3.0×105L·mol-1·cm-1,最大吸收波长为365 nm,测定5.0μg/50 mLSO2-3 6次,RSD为1.8%,线性范围为0~30μg/50 mL,方法应用于食品中SO2-3 的测定。     

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。     

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.     

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.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.