2-Amino-4-bromobutanoic Acid

(2S)- and (2R)-2-Amino-4-bromobutanoic acid were prepared starting from N-Boc-glutamic acid α tert-butyl ester. The double tert-butyl protection was necessary to prevent a partial racemisation during Barton’s radical decarboxylation used to transform the γ-carboxylic group into a bromide. This bromide reacted with different nitrogen, oxygen and sulphur nucleophiles to give nonnatural amino acids characterised by basic or heterocyclic side chains. The title compound was also used to prepare a conformationally constrained peptidomimetic.     

Synthesis of 2•,3•-Dideoxy-3•-<Emphasis Type="Italic">C</Emphasis>-hydroxymethylcytidine Phosphonomethyl Derivatives

Phosphonomethyl substituted 2?,3?-Dideoxy-3?-C-hydroxymethylcytidines have been synthesized and evaluated for their anti HIV-1 activities. The sugar moiety was synthesized starting from (S)-5-hydroxymethylfuran-2-(5H)-one using photocatalyzed addition of methanol. Reduction of the lactone, condensation with silylated 4-methoxy-2(1H)pyrimidinone, followed by phosphonomethylation and deprotection gave the title compounds. The compounds were tested for inhibition of HIV-1 activity but did not show any significant antiviral activity.     

Hydroformylation of Olefins Catalyzed by Rhodium Trichloride Anchored on Ti-HMS

Rhodium trichloride supported on Ti-hexagonal mesoporous silica (Ti-HMS), via a bipyridyl group, is an efficient catalyst for the hydroformylation of olefins at 120 °C and 40.8 atm of CO/H₂ (CO/H₂=2/1). The catalyst is selective leading to high ratios of linear or branched aldehydes from functionalized olefins, and high activity in the case of propene which gave a turnover frequency of 6209 mol/mol(Rh)/h.     

Nucleosides. Part LX. Synthesis and Characterization of Monomeric Cordycepin-Vitamin and Cordycepin-Lipid Conjugates Model Substances for Biodegradable Ester and Carbonate Linkages in Conjugates and Potential Inhibitors of HIV-1 Replication

Monomeric 3′-deoxyadenosine (cordycepin) was modified at the 2′-O- ( 13–18 ) and 5′-O-position ( 25–29 ) by the vitamins E, D₂, and A and by the two lipids 1,2-di-O-palmitoylglycerol and 1,2-di-O-hexadecylglycerol via succinate or carbonate linkages. The base-labile conjugates afforded protection groups like the 2-(4-nitro-phenyl)ethoxycarbonyl (npeoc) and monomethoxytrityl group (MeOTr) that are cleavable without harming the ester and carbonate bonds, respectively. Monomeric conjugates of cordycepin and vitamin E, vitamin D₂, 1,2-di-O-palmitoylglycerol, and 1,2-di-O-hexadecylglycerol (see 13, 14, 17, 18, 25, 26, 28 , and 29 ) inhibited HIV-1-induced syncytia formation 1.7 to 6.2 fold compared to 1.5-fold for cordycepin (see Table); IC₅₀ values for 25 and 28 were 257 and 267 m?M , respectively. In addition, the monomeric cordycepin-vitamin and -lipid conjugates inhibited HIV-1 RT activity 28–49% which compares with a 13% inhibition of HIV-1 RT observed for cordycepin. The minimal inhibition of HIV-1-induced syncytia formation and HIV-1 RT activity did not proceed by the activation of RNase L. The monomeric conjugates tested ( 13, 14 ) increased PKR expression.     

成人血清元素相关性及比值分析

用ＩＣＰ－ＭＳ法测定了７９例成人血清１４种元素水平,并进行了相关分析。结果提示,多种元素间存在显著正相关;分析了部分元素的比值,为相关研究提供了参考范围,且对元素比值的离散程度进行分析,为多元素关系研究提供了新的线索与依据。     

V2O5电致变色薄膜的Raman光谱

近年来,通过向过渡金属氧化物薄膜注入Ｌｉ 制作可调节光透过率的电变色器件已越来越引起广泛的重视[1、2].由于Ｖ2Ｏ5薄膜的稳定性差,限制了它在实际中的应用.因此,为了获得变色效率高、稳定性和可逆性能好的Ｖ2Ｏ5薄膜,使用了多种制备方法,如磁控溅射法[3、6]、电化学沉积法[7、8]、溶胶凝胶法[9、10]、旋涂法[11、12]、真空蒸镀法[13、14]等.但是,无论那种方法都要解决Ｖ2Ｏ5本身在Ｈ2Ｏ或醇等的电解质溶液中电致变色时的溶解问题,通常采用控制薄膜的沉积温度或者退火处理来提高薄膜的电致变色性能[3、4、11].为了探明薄膜结构与电致变色…     

热致液晶三元共聚酯酰亚胺的合成与表征

采用直接熔融缩聚方法由１ ,６ － 己撑－ 双（４ － 羟基酞酰亚胺）（ＢＨＰＩ） 、对羟基苯甲酸（ＰＨ ＢＡ） 和对苯二甲酸（ＴＰＡ） 合成一系列三元共聚酯酰亚胺。对聚合物进行示差扫描量热（ＤＳＣ） 、偏光显微镜（ＰＬＭ） 、广角Ｘ－ 射线衍射（ＷＡＸＤ） 等分析表征,结果表明该系列聚合物具有向列型液晶特征。     

热致性共聚酯液晶的研究——以双酚-对苯二甲酸酯为间隔段

热致性共聚酯液晶由于具有优异的热、机械及加工等性能,引起人们对其应用及基础研究的重视。本实验室曾对以不同长度碳链为软间隔段的共聚酯进行了研究,在产物介晶单元含量不高(约20％)时即可表现出明显液晶性。本文选用以双酚A(BPA)或双酚S(BPS)-对苯二甲酸酯为间隔段进行了研究。     

Chemische Vitamin D<Subscript>3</Subscript>-Bestimmung in Lebertran

The different aspects of Vitamin D₃ determination and the data reported in the literature are discussed. The spectrophotometric determination of Vitamin D₃ in cod-liver oil is carried out after the alkaline saponification, extraction of unsaponified parts, precipitation of accompanying sterols and the column- and thin-layer chromatographic purification and separation of vitamin D₃ on 40 cm plates from other vitamins. The dyestuff α-naphtholbenzein is suited well as standard substance for the better location and identification of vitamin D₃ zone on the thin-layer plate. The results obtained from the chemical method were checked through the simultaneous biological determination.     

Trennung,Identifizierung und Bestimmung von Bactericiden auf der Basis von halogenierten Aromaten mittels Gas-Chromatographie

The separation of a mixture of 22 bactericides has been achieved by gas chromatography on columns with silicone rubber W-982 as stationary phase with temperatures between 100° and 300°C. The unchanged compounds as well as their silylation products have been used. The latter are more conveniently used especially for the quantitative determination. To be able to calculate the retention indices after Kovats gas chromatography has been performed isothermally at 180°C for the more volatile compounds and at 250°C for all other bactericides.The retention indices obtained under these conditions are tabulated together with the limits of detection.