10-对硝基苯氧基癸酸合成工艺的改进

对10-对硝基苯氧基癸酸合成工艺进行了改进.以10-溴代癸酸为原料,与甲醇反应生成10-溴代癸酸甲酯,再与对硝基酚钠反应生成10-对硝基苯氧基癸酸甲酯,最后以固定化脂肪酶水解得到10-对硝基苯氧基癸酸.对中间体的折光率和紫外-可见光谱进行分析,并通过紫外-可见光谱1、H-NMR和13C-NMR以及酶分析应用对最终产物进行确证.结果表明,成功合成出目标化合物,总收率达到71.6%.     

Assignment of chemical shifts in benzohydroxamic acid and structure of its silylated derivatives by 15N enrichment

¹⁵N isotopic enrichment was necessary for the unequivocal assignment of the ¹H NMR lines to the protons in the NH–OH fragment of benzohydroxamic acid, BHXA, C₆H₅CONHOH, in dry dimethyl sulfoxide solutions. The assignment [δ(NH) = 11.21, δ(OH) = 9.01, ¹J(¹⁵N,¹H) = 102.2 Hz, ²J(¹⁵N,¹H) <1.5 Hz], which is opposite to that used by other authors, confirms the assignment extended to BHXA by Brown and co‐workers from the spectra of acetohydroxamic acid. The enrichment allowed also assignment of the ²⁹Si lines in the spectra of disilylated benzohydroxamic acid, (Z)‐tert‐butyldimethylsilyl N‐tert‐butyldimethylsilyloxybenzoimidate (2) and (Z)‐tert‐butyldiphenylsilyl N‐tert‐butyldiphenylsilyloxybenzoimidate (3), and confirmed structure of the monosilylated products, N‐tert‐butyldiphenylsilyloxybenzamide (4) and N‐tert‐butyldiphenylsilyloxy benzoimidic acid (5). Copyright © 2003 John Wiley & Sons, Ltd.     

Preparation of nanometer MgO by sol-gel auto-combustion

Nanometer MgO was prepared via a sol-gel auto-combustion technique using magnesium nitrate as raw material and citric acid as chelating agent. IR spectra of the dried gel were used to investigate the structure of the precursors. By studying the different TG curves of magnesium citrate gel prepared by different methods, we found that a combustion process occurred and the nitrate ions acted as an oxidant in the combustion process. TEM photographs of synthesized powders from the sol-gel auto-combustion showed that the crystallites were uniform in size. In addition, the XRD pattern of this sample showed that the particle size was 8.9 nm. The BET curves, in turn, showed that the specific surface of the sample was 26.34 m²/g. The mechanism of the frothing process in restraining agglomeration is discussed. __________ Translated from Journal of East China Normal University (Natural Science), 2007, (2): 52–57 [译自: 华东师范大学学报(自然科学版)]     

硒化蓖麻酸多相脂质体抗癌机理研究

本文用小角ｘ射线射法法对硒化蓖麻酸多相脂质体的抗癌作用从结构和功能上进行了研究。     

甲酸甲酯水解固体超强酸催化剂的研究

固体超强酸作甲酸甲酯水解转化率和对甲酸的催化剂、进料速度、反应温度对甲酸甲酯水解转化率和对甲酸出口浓度的影响，当原料水与酯的摩尔比为１、反应温度１００℃、原料与催化剂的接触时间为１６ｍｉｎ时，甲酸甲酯的转化率为２４．６％（甲酸的出口浓度达１４．５％）。     

中性磷萃淋树脂吸附铼的性能和机理研究ⅢCL－P＿（350）－KReO＿4－HNO＿3体系

本文报道四甲基膦酸二甲庚酸萃淋树脂（ＣＬ－Ｐ＿（３５０）从硝酸溶液中吸附鳞的性能和机理研究。实验结果表明，吸附平衡服从Ｌａｎｇｍｕｉｒ经验等温式。测得吸附物分子中Ｐ（３５０）与Ｒｅ（Ⅶ）的摩尔比为２：１。Ｒｅ（Ⅶ）是以形式被树脂吸附，其吸附机理属于综合反应：并测定了吸附过程的热力学函数。     

Influence of humic substances on sorption and methylation processes of inorganic- and organo-tin species

The influence of humic substances on sorption and methylation processes for inorganic- and organotin species is presented. Four sediment samples from different locations of the Rivers Elbe, Mulde and Spittelwasser, Germany, with different organotin and humic contents were selected to extract the humic and fulvic acids. The various fractions—the original sediment, the humic acid, the fulvic acid and the residual sediment—were analysed for their organotin content. The individual buyltin species show quite different distribution patterns. Monobutyltin is found mostly associated with humic acids. Dibutyltin shows a nonunique behaviour. At low total organotin content, dibutyltin is found bonded to humic and fulvic acids, whereas at high organotin content dibutyltin is distributed more with the residual sediment. Most of the tributyltin remains in the sediment unextracted; only small quantities of it are in the fulvic acid fraction. Tetrabutyltin is only in the humic acid fraction when it binds to humic matter; it mostly remains in the sediment. General observations indicate that ionic butyltin species bind to fulvic acids whereas the non-polar tetrabutyltin is not found in the fulvic acid fractions in any of the samples. The appearance of monomethyl- and dimethyl-tin species in the humic and fulvic acid fractions after the alkaline extraction was surprising. There is a correlation between the humic content of the sample and the formation of methyltin species. Evidence is provided by experiments that humic substances act as methylation agents.     

聚丙烯酸接枝聚甲基丙烯酸甲酯共聚物的表面性质及粘度性质的研究

聚丙烯酸接枝聚甲基丙烯酸甲酯共聚物的表面有其特殊性质:水滴在其表面上形成的接触角基本上与其组成无关,而丙烯酸——甲基丙烯酸甲酯无规共聚物的表面接触角却与其组成有密切关系;接枝共聚物在DMF溶液中,其粘度表现出有趣的现象,说明了接枝共聚物在溶液中有微区现象和聚电解质性质     

乳清酸的2.5次微分示波极谱法测定

拟定了乳清酸的2.5次微分示波极谱测定新方法.结果表明在0.8 mol/L HCl介质中,乳清酸产生一灵敏的极谱还原波,峰电位Ep =-0.77 V(vs.SCE);其2.5次微分极谱峰峰电流ep″与乳清酸浓度在4.0×10-8～4.0×10-5 mol/L范围内呈良好线性关系(r=0.999 6,n=9),检测限为1.0×10-8 mol/L;13次平行测量4.0×10-7 mol/L乳清酸的峰电流,所得RSD为1.8%.该方法可直接用于测定牛奶中乳清酸的含量.