异丙烯膦酸的合成及表征

本文以三氯化磷（ＰＴ），丙酮（ＡＬ）和冰醋酸（ＡＡ）为原料合成了异丙烯膦酸（ＩＰＰＡ），详细探讨了原料配比、反应温度和反应时间对产物收率的影响，并用红外光谱、３１ＰＮＭＲ、１ＨＮＭＲ和１３ＣＮＭＲ证实了产物的结构。     

过渡金属离子与氨基酸形成配合物的NMR研究

氨基酸是生命系统中蛋白质的基本结构单位,生物分子中的氨基酸是金属离子重要的配位体之一。我们测定了甘氨酸、精氨酸等六种氨基酸与金属离子Zn~(2+),Cd~(2+),Hg~(2+)的~1H和~(13)C NMR谱,从而探讨它们的配位机理。实验结果表明,在加入过渡金属离子前后,氨基酸的~1H和~(13)C谱的化学位移位发生了一定的变化,据此可揭示过渡金属离子和氨基酸形成配合物的配位点,进而可研究所形成配合物的结构及其成键规律。     

含吡啶氮杂套索冠醚Ⅰ与Ba~(2+)配位的NMR研究

冠醚与碱金属、碱土金属有良好的配位作用,氮原子取代冠醚的部分氧原子,可改善它与过渡金属的配位能力,套索冠醚既有简单单环冠醚的动态性质,又有窝穴体分子的三维键合特征,因而进一步提高了其配位能力及配位选择性。目前,氮杂套索冠醚的NMR研究已引起人们的重视,但氮杂套素冠醚与金属离子配位的NMR研究尚不多见。本工作使用VarainXL-200超导谱仪对新合成的含吡啶氮杂套索冠醚(结构见图1)与Ba~+的配位进行了探     

Protein NMR in biomedical research

Nuclear magnetic resonance (NMR) spectroscopy is a versatile biophysical technique with wide applicability in drug discovery research, particularly for the detection and characterization of molecular interactions. This review highlights in a comprehensive manner the aspects of biomolecular NMR which are most beneficial for pharmaceutical research and presents them as contributions to the different stages of a drug discovery program: target selection, assay development, lead generation and lead optimization. Emphasis is put on the concept of the particular NMR application, rather than on technical details, and on recent examples. Finally, an appendix of frequently asked questions is given.Received 7 October 2003; received after revision 11 November 2003; accepted 27 November 2003This revised version was published online in September 2004. In the previous version, the authors were listet in reverse order.     

Effect of total aluminum concentration on the formation and transformation of nanosized Al13 and Al30 in hydrolytic polymeric aluminum aqueous solutions

Influence of total aluminum concentration （CAIT） on the generation and transformation of nanosized AI13 and AI30 in hydrolytic polyaluminum aqueous solutions was investigated using high field 27AI NMR and time-developed AI-Ferron complex colorimetry. When prepared at the optimal basicity （B） of Al13 generation and 80℃, the All3 species in polyaluminum solution tends to further polymerize and convert to AI30 and higher polymers when CAI; 〉0.2 mol· L^-1, but Al13 does not convert to AI30 quantificationally, as the formation of Alu from Al13 and AI30 is accelerated in the same way. The conversion rate of All3 is accelerated by the increase in CAIT. When CAlT 〉0.75 mol·.L^-1, Al13 content decreases rapidly, and AI30 content increases continuously and becomes the dominant nanometer polynuclear aluminum species. AIm is one of prerequisites of Al13 conversion to AI30. When CAI; increases and B reduces, the polymerization rate between Al13 and Aim increases, and at the same time, the dissociation reaction rate of All3 and AI30 by H^＋ also increases. The latter becomes the dominant reaction in polyaluminum solution with low B value, so AI30 decreases with the increasing CAlT. The hydrolytic polyaluminum solution with Al13 content beyond 80% can only be prepared under the condition of CAlT〈0.5 mol· L^-1 and optimal B value.     

三种(1,10-二甲氧基)-11-萘甲烷基醚的制备、表征及理论研究

报导了标题化合物的制备，测定了标题化合物的核磁共振谱．并用HF/4-31G方法优化了三种化合物构型，在此基础上再用GMO从头计算方法计算了三种化合物的MNR谱，其结果与实验值符合较好，显然，NMR的量子化学计算可为确定化合物的结构提供一种新的工具。     

八氯二丙醚的合成和二维核磁谱研究

八氯二丙醚由三氯乙烯和氯甲醚或甲醛制备。产物的结构由＾１ＨＮＭＲ，＾１３ＣＮＭＲ，ＤＥＰＴ谱、二维核磁＾１３Ｃ－＾１Ｈ相关谱，ＣＯＳＹ谱、质谱、红外谱和元素分析确定。     

α-二苯基膦羰基化合物的合成及还原制醇

介绍了用二本基膦三甲基硅烷与α-氯代或溴代酮反应合成α-二苯基膦苯乙酮(Ⅰ)、二苯基膦甲基-β-萘基酮溴化物(Ⅲ)、二苯基膦甲基-1-金刚烷基酮溴化物(Ⅴ)等新化合物.用二苯基氯膦与乙酸乙酯烯醇锂盐反应制备α-二苯基膦乙酸乙酯(Ⅵ);用四氢铝锂还原羰基化合物制备相应的仲醇;酯Ⅵ与甲基溴化镁反应制得二苯基膦叔丁醇(Ⅶ).并对各化合物的~(13)C和~(31)P核磁共振谱作了研究.