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高纯度萘呋胺酯草酸盐的制备及其某些单晶分子结构
引用本文:薛敏,汪进良,余伟发,王道林,章军,周智明. 高纯度萘呋胺酯草酸盐的制备及其某些单晶分子结构[J]. 北京理工大学学报, 2002, 22(5): 658-661. DOI: 10.3969/j.issn.1001-0645.2002.05.033
作者姓名:薛敏  汪进良  余伟发  王道林  章军  周智明
作者单位:北京理工大学,化工与材料学院,北京,100081
摘    要:根据英国药典(1998版)萘呋胺酯草酸盐质量标准要求,采用柱层析、高真空蒸馏、重结晶等化学及物理手段以及不同工艺相结合的方法,降低杂质含量,经HPLC分析表明:采用高真空蒸馏和水重结晶相结合的方法可使产品质量达到英国药典要求,最终得到主产品质量分数高达99.6%以上的高纯度萘呋胺酯草酸盐;并首次报道了萘呋胺酯草酸盐两个非对映异构体单晶分子结构.

关 键 词:萘呋胺酯草酸盐  杂质  HPLC  柱层析  高真空蒸馏  单晶结构
文章编号:1001-0645(2002)05-0658-04
收稿时间:2001-12-18
修稿时间:2001-12-18

Preparation of Highly Purified Nafronyl Oxalate and Its X-Ray Single Crystal Structure
XUE Min,WANG Jin-liang,YU Wei-f,WANG Dao-lin,ZHANG Jun and ZHOU Zhi-ming. Preparation of Highly Purified Nafronyl Oxalate and Its X-Ray Single Crystal Structure[J]. Journal of Beijing Institute of Technology(Natural Science Edition), 2002, 22(5): 658-661. DOI: 10.3969/j.issn.1001-0645.2002.05.033
Authors:XUE Min  WANG Jin-liang  YU Wei-f  WANG Dao-lin  ZHANG Jun  ZHOU Zhi-ming
Affiliation:School of Chemical Engineering and Materials Science, Beijing Institute of Technology, Beijing100081, China;School of Chemical Engineering and Materials Science, Beijing Institute of Technology, Beijing100081, China;School of Chemical Engineering and Materials Science, Beijing Institute of Technology, Beijing100081, China;School of Chemical Engineering and Materials Science, Beijing Institute of Technology, Beijing100081, China;School of Chemical Engineering and Materials Science, Beijing Institute of Technology, Beijing100081, China;School of Chemical Engineering and Materials Science, Beijing Institute of Technology, Beijing100081, China
Abstract:Several different technological processes, including that of high vacuum fractionation, column chromatography and recrystallization, have been tried to reduce the quantity of impurities contained in the raw nafronyl oxalate. HPLC analysis showed that a combination of high vacuum distillation and water recrystallization led to a high quality product (99.6% purity), meeting the British Pharmocoepia (1998) standard. X-ray single crystal analysis confirmed the structure of the title compound as first reported.
Keywords:nafronyl oxalate  impurity  HPLC  column chromatography  high vacuum distillation  single crystal structure
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