蜜胺甲醛树脂-钯催化剂的制备及其催化氢解氯代苯基中间体合成多西紫杉醇及其异构体侧链的研究  

PREPARATION AND CATALYTIC HYDROGENATION OF MELAMINE FORMALDEHYDE RESIN-Pd FOR CHLOROPHENYL COMPOUNDS AND SYNTHESIS OF SIDE CHAIN OF DOCETAXEL

作　　者：齐传民[1] 游桂荣[1] 杨凌春[1] 孙彭利[1] 

机构地区：[1]北京师范大学化学系,北京100875

出　　处：《化工科技》2003年第1期1-5,共5页Science & Technology in Chemical Industry

基　　金：国家自然科学基金资助课题(20171008)

摘　　要：制备和表征了蜜胺甲醛树脂钯催化剂,通过光电子能谱、顺磁共振谱和X 射线衍射等测试证明新催化剂与Pd2+络合,起催化作用的是Pd0,研究发现催化剂的N/Pd原子比在25.6～12.8具有较好的催化效果,而催化氢化温度则在35～40℃之间进行更好。蜜胺甲醛树脂的聚合度越高对钯的附载能力越强,催化剂的催化效果越好。该催化剂在常压和室温条件下将氯代苯基化合物催化氢化为苯基化合物,并有很高的催化活性,通过该方法以较高收率制备了多西紫杉醇和异构体侧链。得到的新化合物均经过1HNMR、13CNMR、IR、旋光度和元素分析等给予确证,(3S,4R) 3 羟基 N [(S) (1 苯基)乙基] 4 (2′ 氯苯基) 2 氮杂环丁酮通过X 单晶衍射确定四元环构型为3S,4R型,并进一步确定了其它化合物的结构。?Melamine formaldehyde resinPd complex as hydrogenation catalyst has been studied by XPS,EPMA XRD and ESR.The results showed that the oxidation states of the palladium were 2+(Pd2+) in the fresh catalyst and 0 (Pd0) in the used catalyst.The influence of temperature and the N/Pd atomic ratio in the catalyst on the effects of hydrogenation was measured and the optimum conditions were found.The higher degree of polymerization of melamine formaldehyde resin in the catalyst had better influence to catalyst activity.It had high catalytic hydrogenation activity to chlorophenyl compounds to phenyl compounds at room temperature under atmosphere pressure.Side chains of Docetaxel were obtained by this method in higher yield.Novel chloro phenyl azetones and their reduced compounds,2hydroxyl3amino3chlorophenyl propyl propionate were identified on the basis of the spectroscopic data,such as IR,1HNMR,13CNMR,MS or elementary analysis. 

关 键 词：催化氢化 蜜胺甲醛树脂 多西紫杉醇 Staudinger环加成反应 氮杂环丁酮 

分 类 号：TQ464.9[化学工程—制药化工] TQ426.94