脱羧氯雷他定的合成

脱羧氯雷他定 (ＤＣＬ)是一种有效的非镇定性抗组织胺 ,对过敏性鼻炎 ,糖尿病、咳嗽、普通感冒、流行性感冒、关节痛及其它不适症状都有很好的疗效[1～2 ] 。它克服了氯雷他定、酮康唑、红霉素、伊曲康唑等易引发黑色素瘤、纤维肉瘤、胃刺激、肥胖症、心律失调、传导紊乱等症状的缺点。且它的使用剂量只有氯雷他定的十分之一 ,有很好的市场前景和实际应用价值。ＭａｒｋＷ .Ｈｏｌｌａｄａｙｅｔａｌ[3] 在水溶液中由酸、碱催化得到了脱羧氯雷他定 ,但无具体操作和反应结果报道。Ａ .Ｋ .ＧｕｎｎａｒＡｂｅｒｇ[1] 直接用ＫＯＨ在绝对无水…     

2-氰基-3-甲硫基-3-取代甲氨基丙烯酸酯类化合物的合成及其除草活性

A series of 2-cyano-3-methylthio-3-substituted methylaminoacrylates were synthesized as herbicidal inhibitors of photosystem Ⅱ （PSⅡ） electron transport, in order to estimate the effect of fluorine atom, pyridyl group, chirality and ester chain on activity. The important intermediate 2-fluoro-5-aminomethylpyridine was synthesized with high yield. The bioassay results showed that most of rifle compounds had high herbicidal activity in postemergence treatment. The introduction of an a-methyl into the 3-substituted methylamino could improve the activity notably. The replacement of hydrogen by chlorine or fluorine group and phenyl by pyridyl group showed different effects, and at the same time, the ester chain affected the activity too.     

示波极谱法测定保健食品中维生素B1

在pH 5.0的柠檬酸盐缓冲溶液及0.15 mol·L-1KCl底液中,维生素B1在-1.40 V处出现灵敏的极谱波,据此提出了测定保健食品中维生素B1的快速而灵敏的示波极谱法.在pH4.7～5.2的范围内,可得到对称的二阶导数峰.峰电流(ip)与维生素B1浓度在0.1～8.0 mg·L-1间呈线性关系,其检出限为0.078 mg·L,连续测定6天,每天测定6次,对方法的精密度作了检验,所得结果的日内RSD值小于4.78%,日间RSD值为5.76%,回收率的测得值在92.0%及107.2%之间,对五种保健食品,用此法及国家标准法分别测定,所得分析结果用t-检验法进行检验,表明相互间无显著差异(t=1.76,P＞0.05).     

Design and Synthesis of 1-Benzyl-3-(a-hydroxy-(un)substituted benzylidene)pyrrolidine-2,4-diones as Potential Herbicides

The inhibitors of 4-hydroxyphenylpyruvate dioxygenase (HPPD, EC 1.13.11.27) are an new kind of herbicides.[1]Generally, in structure, potent herbicides of this kind must possess: (1) a tricarbonyl methane structure and one of the three carbonyl groups must be a subustituted benzoyl group; (2) the compound must be able to enolise so that the enolate is capable of inhibiting HPPD enzyme by competitive combination with Fe2+, the reaction center of HPPD enzyme.[2]Recently, we noticed that the 3-acyltetramic acids form an expanding group of antibiotics and pigments from micro-organisms,[3] they display a range of biological activities[4] and all of this kind compounds possess all of the characters mentioned above. Tests of their antimicrobial activities indicated that the structure of the acyl substituent at the 3-position was important to many typical antibiotics.[4～6] These characters stimulated us to study this kind of compounds so as to discover new herbicides. In this report, we synthesized a series of compounds 3 and tested their herbicidal activities to investigate their structure-activity relationships.     

A New Cyclohexene Oxide from Uvaria tonkinensis var. subglabra

A new compound, subglain B, was isolated from the stems of Uvaria tonkinensis var.subglabra and its structure was identified as 1S, 2R, 3S, 6R-1-benzoyloxymethylene-1,2-dihydroxy-3-benzoyloxy-6-chlorocyclohex-4-ene (1), by spectral evidences.     

Synthesis and Asymmetric Enantioselective Addition of Chiral Polybinaphthyl and Polybinaphthol I.igands

Four chiral polymers P-1, P-2, P-3 and P-4 were synthesized by the polymerization of （S）-2,2＇-dioctoxy-1,1＇- binaphthyl-6,6＇-boronic acid （S-M-3） with （S）-6,6＇-dibromo-1,1＇-binaphthol （S-M-1）, （R）-6,6＇-dibromo-1,1＇- binaphthol （R-M-1）, （S）-3,3＇-diiodo-1,1＇-binaphthol （S-M-2） and （R）-3,3＇-diiodo-1,1＇-binaphthol （R-M-2） under Pd-catalyzed Suzuki reaction, respectively. All four polymers can show good solubility in some common solvents due to the nonplanarity of the polymers in the main chain backbone and flexible alkyl groups in the side chain. The analysis results indicate that specific rotation and circular dichroism （CD） spectral signals of the alternative S-S chiral polymers P-1 and P-3 are larger than those of S-R chiral polymers P-2 and P-4, but their UV-Vis and fluorescence spectra are almost similar. The results of asymmetric enantioselectivity of four polymers for diethylzinc addition to benzaldehyde indicate that catalytically active center is （R） or （S）-1, 1＇-binaphthol moieties.     

CuI催化的酰胺和溴苯的偶联反应研究

本文报道了一种新的催化体系 (CuI / 氨基酸 / K₃PO₄) 催化胺和芳香溴代化合物之间的交叉偶联反应，对于不同的底物都以较好的产率得到了产物。该反应操作简单，适用性广，并且试剂价格便宜。     

Enhancement of Photocurrent Generation of a Novel Stilbazolium Dye Dimer in LB Monolayer Films

A novel dye dimer,bis-{[1-(N-hexadecyl-4-pyridinium)-2-(4-N,N-dimethylaminopheyl)] ethenyl} methane diiodide (C16BP) was synthesized,and the photoelectrochemistry of the dye Langmuir-Blodgett monolayer modified ITO electrode was investigated.For comparison,the photoelectrochemistry of the monomer (E)-N-hexadexyl-4-[2-(4-N,N-dimethylaminophenyl) ethenyl] pyridinium iodide (C16P) was also measured.The results show that the photocurrent generation property of the dimer is enhanced.The photocurrent generation quantum yield is 0.38% for C16BP,while that for C16P is 0.23%.     

基于碳纳米管的化学修饰电极及电化学生物传感器的研究进展

综述了碳纳米管的结构、合成、纯化、功能化、分散及基于碳纳米管的化学修饰电极和电化学生物传感器的研究进展。     

微波衍生-离子对高效液相-磺化四苯基卟啉光度法同时测定痕量镍、铜、锰和锌

 用磺化四苯基卟啉 (TPPS4 )作柱前衍生试剂 ,在微波作用下进行衍生反应 ,研究了衍生和分离Ni2 + ,Mn2 + ,Zn2 + 和Cu2 + 的最佳条件。在 75 0W的微波作用下衍生反应 3min ,在C18柱上采用乙腈 水 (体积比为 2 2 5∶77 5 )体系作流动相 ,四乙基溴化铵 (TEABr)作离子对试剂 ,在 415nm处检测 ,建立了微波衍生 离子对高效液相快速分离、光度检测Ni2 + ,Mn2 + ,Zn2 + 和Cu2 + 的新方法。络合物和反应试剂在 15min内出峰完毕。Zn2 + ,Cu2 + ,Ni2 + 和Mn2 + 的检测限分别为 0 0 5 μg/L ,0 0 1μg/L ,0 10 μg/L和 0 40 μg/L。