摘要
本文对雷尼替丁的传统合成方法进行优化和改进,提高了产物的收率和纯度。氮气保护下,以蒸馏水为溶剂,将N-甲基-1-甲硫基-2-硝基乙烯胺(简称侧三)和2-[[[5-(二甲氨基)甲基-2-呋喃基]甲基]硫基]乙胺(简称氨乙基硫醚)按照摩尔比1.156∶1投料,36℃下反应4h,反应结束后将反应液调酸至p H 3.5~4,经二氯甲烷萃取,有机相回收侧三,回收率高达98.9%;水相调碱至p H 9~10,经萃取、干燥、过滤、浓缩、重结晶,得到雷尼替丁,收率最高达89.7%。
The traditional chemical synthesis methods have been optimized to get high yield and purity of ranitidine in this paper. Under the protection of nitrogen, N-methyl-1-alkylthio-2-nitroethenamines （referred to as “three side”） and 2-[[[5-（dimethylamine）methyl-2-furanyl]methyl]thio]ethylamine（referred to as“thiobisethylamine”） as raw material in the mole ratio of 1.156：1 was added to the water, keep the temperature at 36 ℃ for 4 h. The reaction mixture can be acidified to a pH= 3.5~4 and extracted with dichloromethane. The organic phase can be used to recycle three side with high recovery rate of 98.9%. Water phase can be basified to a pH=9~10, then it was extracted with dichloromethane again, dried, filtered, evaporated, recrystallised to get the ranitidine with yield of 89.7% and melting point of 68-70 ℃.
作者
刘磊
王丽丽
吕海军
康彩红
Wang Lili Lv Haijun Kang Caihong(Hebei Research Center of Pharmaceutical and Chemical Engineering, College of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang 050018 Hebei Key Laboratory of Molecular Chemistry for Drug, Hehei Research Center of Pharmaceutical and Chemical Engineering, Shijiazhuang 050018)
出处
《化学通报》
CAS
CSCD
北大核心
2017年第2期212-215,共4页
Chemistry
基金
国家自然科学基金项目(21102032)
北京分子科学国家实验室开放基金(20140120)
河北省自然科学基金(B2014208121)
河北省教育厅项目(Z2013001)
河北科技大学五大平台开放基金项目(2015PT37)资助
