| 刘磊,王丽丽,吕海军,康彩红.化学通报,2017,80(2):212-215. |
| 雷尼替丁的合成及工艺研究 |
| The synthesis of ranitidine and its process research |
| 投稿时间：2016-08-11 修订日期：2016-09-17 |
| DOI： |
| 中文关键词: 侧三回收 氨乙基硫醚 雷尼替丁 |
| 英文关键词:synthesis three side thiobisethylamine ranitidine |
| 基金项目: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)和河北科技大学五大平台开放基金项目(2015PT37)资助 |
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| 中文摘要: |
| 本文对雷尼替丁的传统化学合成方法进行优化和改进,提高了收率和纯度。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,对反应液调酸至 pH=3.5~4,经二氯甲烷萃取,得到有机相和水相。有机相回收侧三,回收率高达98.9%。水相调碱至pH=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%,熔点：68-70℃。 |
| 英文摘要: |
| 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 ℃. |
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