改性环糊精气相色谱手性固定相拆分对映体的选择性及拆分机理的讨论

改性环糊精气相色谱手性固定相拆分对映体的选择性及拆分机理的讨论周昕，万宏，欧庆瑜（中国科学院兰州化学物理研究所兰州７３００００）１前言自１９８８年Ｋｏｎｉｇ￣［１］等人成功地将改性环糊精用于毛细管气相色谱固定相拆分对映体以来，环糊精衍生物以其高选择性...     

Design and Synthesis of Glycosylated Aromatic Nitrogen Mustard Derivatives

Antibody-directed enzyme prodrug therapy(ADEPT) is a new strategy for the treatment of cancer that has arisen in recent twenty years, the main merits of which are that it can improve the selectivity of anticancer drugs and reduce the side effects in remote tissue. In the present study, two prodrugs-glycosylated aromatic nitrogen mustard derivatives were synthesized. Glucose and lactose were converted into glycosyl donors-trichloroacetimidate; the obtained glycosyl donors were glycosylated with p-nitrophenol(glycosyl donors) to form β-glucosyl p-nitrobenzene and β-lactosyl p-nitrobenzene that were protected by acetyl in a stereoselective manner; the two products were reduced by zinc dust and then treated with ethylene oxide, afforded two glycosylated nitrogen mustard derivatives that were protected by acetyl; the last step was to deacetylate and then afforded the two target compounds that could be used as prodrugs of ADEPT for further Anti-tumor research.     

酰胺衍生物型手性固定相拆分普萘洛尔对映体

１引言普萘洛尔（ｐｒｏｐｒａｎｏｌｏｌ）是临床使用的一种β－受体阻滞剂，由于其对映体在药理和药物动力学方面存在差异，所以它的拆分工作具有重要意义。本文首次用酰胺衍生物型手性固定相正相直接拆分普萘洛尔对映体，优化了分离条件，拆分过程直接、快速、有效。最后推断了对映体的洗脱顺序。２实验部分２．１仪器与试剂Ｖａｒｉａｎ５０００型液相色谱仪，ＵＶ－１００型紫外可见分光检测器。所用试剂为分析纯（重蒸）。盐酸普萘洛尔（北京第二制药厂）经如下处理：取适量盐酸普萘洛尔，加入２ｍＬ１，２－二氯乙，再加入１ｍＬ１．…     

Synthesis of Calix[4]arene Derivatives with NLO Properties

The new chromophore compounds with NLO properties were prepared by Knoevenagel condensation from forrnyl or diformyl calix[4/arene and isophorone derivatives in the presence of piperidine and acetic acid, respectively. In these chromophore calix[4]arenes, the ring locked trienes were employed as the conjugation bridge and electron acceptor in D-π-A units. The NMR spectra demonstrated that they existed in a cone conformation and consequently non-conjugated D-π-A units could be oriented at nearly the same direction.     

β－环糊精含硫衍生物自组单分子膜修饰金电极的选择穿透性研究

β－环糊精含硫衍生物自组单分子膜修饰金电极的选择穿透性研究何品刚，方禹之，铃木，嚴长，哲郎（华东师范大学化学系，上海，２０００６２）（东北大学药学部，仙台９８０，日本国）关键词硫辛酰－β－环糊精衍生物，自组单分子膜，金电极近年来，为在分子水平上控制和...     

含羟基芳基或氨基芳基的磷酰胺酯衍生物的合成

采用均相反应的方法合成了6个含羟基芳基或氨基芳基的磷酰胺酯衍生物:[(ClCH_2CH_2)_2NP(O)(OPh)(XArY)](X:O,NH;Y:m或p-OH或NH_2).用元素分析、红外光谱、氢核磁共振谱及质谱证实了它们的组成及结构.     

碳纤维微电极研究(Ⅺ)——利用温度效应测定电极反应的热力学和动力学参数

研究了温度对碳纤维微电极上伏安曲线的影响及温度与电极电位的关系,测定了电极反应的热力学参数.由电流与温度的关系测定了去极剂的扩散活化能E_(al)和D_o,利用微电极具有高速传质的特性,测定了常规电极上为可逆反应的电极反应标准速率常数(?),并通过(?)与温度的关系测定了电极反应的活化能.     

Synthesis of 2-Aminochromene Derivatives Catalyzed by KF／Al2O3

A series of 2-aminochromene derivatives including 2-amino-ben-zo[ h ] chromene, 2-amino-benzo [ f ] chromene and 2-amino-pyrano [3,2-h ]quinolin derivatives was synthesized from aryl-aldehyde, malononitrile or ethyl cyanoacetate and 1-naphthol or 2-naphthoi or 8-hydroxyquinoline in refluxing ethyl alcohol cat-alyzed by KF-Al2O3. The structures were confirmed by X-ray analysis.     

系列单取代烷氧基-2-羟丙基-β-环糊精的合成与表征

以环氧氯丙烷和脂肪醇为原料, 通过相转移催化法合成了乙基、正丙基、正丁基和正戊基缩水甘油醚(1～4), 并利用所合成的缩水甘油醚和β-环糊精为原料, 分别在弱碱水溶液(1.5%)和强碱水溶液(30%)中制备并用硅胶柱分离出单2位取代的乙氧基、丙氧基、丁氧基和戊氧基-2-羟丙基-β-环糊精(1a～4a)和单6位取代的丙氧基、丁氧基和戊氧基-2-羟丙基-β-环糊精(2b～4b), 利用薄层色谱、红外光谱、差热扫描量热分析、质谱和核磁共振等手段对所合成的产品进行了表征.