光活性酮咯酸衍生物的拆分及绝对构型的测定  

The Resolution of the Optical Active Derivatives of Ketorolac and the Determination of its Absolute Configuration

作　　者：宁家成[1] 杨鳌[1] 关烨第[1] 王哲明[2] 严纯华[2] 

机构地区：[1]北京大学化学与分子工程学院 [2]北京大学稀土材料化学与应用国家重点实验室,北京100871

出　　处：《物理化学学报》2002年第9期821-824,共4页Acta Physico-Chimica Sinica

摘　　要：酮咯酸与L-脯氨酸苄酯在缩合剂作用下形成酰胺,用柱层析分离了一对非对映异构体并进行了表征.用单晶X衍射测定了酮咯酸脯氨酸苄酯酰胺一个异构体的晶体结构,并用内参法确定了其绝对构型.晶体属正交晶系,空间群P212121,晶胞参数a=0.89645(1)nm,b=1.27123(2)nm,c=2.07621(4)nm,V=2.36604(6)nm3,Z=4,最终偏离因子R1=0.0464.A pair of diastereoisomer of Pro Obzl of keterolac amide, formed by the reaction of(±) ketorolac and L proline under the action of condensation agent,were resolved using column chromatography and characterized by 1H NMR, 13C NMR, IR, MS spectra and elemental analysis. The crystal structure of one diastereoisomer of the amides was determined by single crystal diffraction analysis, and the absolute configuration of which was deduced by internal reference. The crystal belongs to orthorhombic space group P212121. Crystallographic data are:a=0.896 45(1)nm, b=1.271 23(2)nm,c=2.076 21(4)nm, V=2.366 04(6)nm3, Z=4, R1=0.0464.

关 键 词：光活性酮咯酸衍生物 测定 非对映异构体 拆分 晶体结构 绝对构型 消炎镇痛药 

分 类 号：TQ460.7[化学工程—制药化工]