摘要
目的研究二去水卫矛醇的合成工艺。方法以植物提取的卫矛醇为起始原料,在0.16 mol·L-1溴酸溶液中进行溴代反应得到二溴卫矛醇(DBD),DBD和碳酸钾在叔丁醇中发生分子内消除反应得到二去水卫矛醇(DAG)粗品,经重结晶得到DAG纯品,并采用正交实验设计法对实验中所涉及的温度、溶剂用量和碱的用量等进行了优化。结果与结论本法原料易得,反应条件温和,后处理简便,适合放大生产,总收率为50%左右,产品纯度和有关物质均符合中华人民共和国药典规定。
Dianhydrogalactitol was synthesized from bromination of natural dulcitol in 0. 16 mol.L-1 hydrobromic acid solution to afford dibromodulcitol, which was subjected to intramolecular elimination with potassium carbonate, followed by recrystallization in n-butanol/acetone with satisfied overall yield. The content of purity and related substances meet the requirements of Chinese Pharmacopeia.
出处
《中国药物化学杂志》
CAS
CSCD
2016年第2期109-111,共3页
Chinese Journal of Medicinal Chemistry
关键词
抗肿瘤药物
二去水卫矛醇
合成
antineoplastic drug
dianhydrogalactitol
synthesis
