有机五价碘氧化试剂

介绍了最近几年有关五价碘氧化试剂在有机合成中应用的研究进展,主要从合成、应用、机理方面进行了阐述。     

Photocatalytic degradation of methylene blue on Fe3+-doped TiO2 nanoparticles under visible light irradiation

Fe³⁺-doped TiO₂ composite nanoparticles with different doping amounts were successfully synthesized using sol-gel method and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and ultravioletvisible spectroscopy (UV-Vis) diffuse reflectance spectra (DRS). The photocatalytic degradation of methylene blue was used as a model reaction to evaluate the photocatalytic activity of Fe³⁺/TiO₂ nanoparticles under visible light irradiation. The influence of doping amount of Fe³⁺ (ω: 0.00%–3.00%) on photocatalytic activities of TiO₂ was investigated. Results show that the size of Fe³⁺/TiO₂ particles decreases with the increase of the amount of Fe³⁺ and their absorption spectra are broaden and absorption intensities are also increased. Doping Fe³⁺ can control the conversion of TiO₂ from anatase to rutile. The doping amount of Fe³⁺ remarkably affects the activity of the catalyst, and the optimum efficiency occurs at about the doping amount of 0.3%. The appropriate doping of Fe³⁺ can markedly increase the catalytic activity of TiO₂ under visible light irradiation. __________ Translated from Journal of Northwest Normal University (Natural Science), 2006, 42(6): 55–56 [译自: 西北师范大学学报(自然科学版)]     

反向流动注射化学发光法测定痕量铁

基于邻菲别名林对高碘酸钾－碱性鲁米诺－铁体系发光强度的增敏作用建立了水体中总铁的反向流动性化学发光检测方法。该法线性范围在１×１０＾－４－１０ｍｇ／Ｌ，检测限为３×１０＾－６ｍｇ／Ｌ，对于５×１０＾－３ｍｇ／Ｌ Ｆｅ测定９次的相对标准偏差为０．９％。此方法已用在水处理中总铁的监测。     

Palladium-catalyzed homocoupling reactions between two Csp(3)-Csp(3) centers

[reaction: see text] A novel palladium-catalyzed coupling reaction between two Csp(3)-Csp(3) centers has been investigated. This protocol is initiated by the oxidative addition of an alpha-halo carbonyl compound to a palladium(0) species, followed by the double transmetalation. The key dialkyl palladium intermediate undergoes reductive elimination to form the desired coupling product.     

胶束增敏导数—可变角同步荧光法同时测定两种羟基联苯

本文建立了２，２’－二羟基联苯（ＤＨＰ）和４－羟基联苯（ＨＰ）的胶束增敏导数－可变角同步荧光同时分析方法，可变角同步扫描所得到的ＤＨＰ和ＨＰ的谱峰位置均对应于常规光谱中的最佳激发－发射位置，经二阶求导后，消除分析谱带干扰，所得的二阶导数－可变角同步光谱即可用于两物质的同时测定，方法快速灵敏，ＤＨＰ测定范围为０．０５～０．５ｍｇ／Ｌ，ＨＰ测定范围为０．０７～２ｍｇ／Ｌ。     

铜膜差分脉冲阳极溶出伏安法测定药物中铋的含量

研究了铜膜电极代替汞膜电极测定重金属铋的差分脉冲溶出伏安法。实验了同位镀膜法测定铋的条件。在最佳实验条件下,Bi3+浓度在5×10-8~2×10-5mol/L范围内,其溶出峰峰高与浓度呈线性关系,检出限达到1×10-8mol/L。测定了一些药物中铋的含量,结果准确。     

Synthesis and Insulin—sensitizing Activity of a Series of 2—Benzyl—1,3—dicarbonyl Derivatives

A series of 2-benzyl-1,3-dicabonyl derivatives was synthesized.Their insulin-sensitizing activity was evaluated in 3T3-L1 preadipocyte cells.Compounds3,26 and 27 were found to possess strong insulin-sensitizing activity in vitro and were selected for further hypoglycemic evaluation in vivo.     

尼龙1010／尼龙6共聚物的表观相图研究

采用显微熔点法和ＤＳＣ测定了尼龙１０１０／尼龙６共聚物的表观相图；分析了投料比与链节结构单元含量的关系。最低熔点时尼龙１０１０／尼龙６的理论重量投料比为６０／４０，摩尔比为３３．３／６６．７，实验结果与此相近。     

Study on open tubular capillary affinity liquid chromatography

A novel mode of affinity chromatography (AC) based on an open tubular capillary column (OTAC) is demonstrated. The OTAC column is prepared by immobilizing Cibacron blue F3GA onto the inner surface of a 50-microm-i.d. capillary column. The AC experiment is performed on a capillary electrophoresis instrument by using its pressure system as the driving force. Bovine serum albumin and lysozyme (Lys) are successfully separated with stepwise gradient elution. The relative standard deviation (RSD) for the elution time of the retained Lys is 0.08%, and good repeatability of its peak area and peak height with an RSD value lower than 2.12% for 10 consecutive runs is observed. The loading capacity and detection limit for the retained Lys are approximately 36 ng and 8.6 ng, respectively. It is also found that the amount of protein adsorbed is unaffected by the flow rate of the loading buffer, and OTAC can be used for the fast determination of biopolymers. Some of the advantages of OTAC over conventional modes of open tubular capillary liquid chromatography are that the detection sensitivity and loading capacity of a sample can be greatly improved, because the relatively large inner diameter of the capillary can be adopted and the whole capillary column can be used to adsorb the solute in OTAC.     

一步法合成N-1,3-二羟基丙烷-2-基烷基乙酰胺

以5-氨基烷基-2,2-二甲基-1,3-二噁烷为起始原料, 乙酸酐为酰化剂, 一步法选择性地合成氨基二醇类氨基乙酰化产物N-1,3-二羟基丙烷-2-基烷基乙酰胺. 该方法操作简便, 收率高. 所合成的4个新化合物的结构均经FTIR, ¹H NMR, ¹³C NMR及HRMS确证. N-3-(1,3-二羟基丙烷-2-基)丙基乙酰胺(1a)作为关键的中间体, 可以用于HIV-1 Tat/ PCAF BRD抑制剂4的合成.