3-苯胺基-2-(3,4,5-三甲氧基苄基)丙烯睛的合成研究

Synthesis and Resarch of 3-(phenylamino)-2-(3,4,5-trimethoxybenzyl)acrylonitrile

甲氧苄啶(TMP)是我国医药行业的支柱产品之一,但关键中间体3-苯胺基-2-(3,4,5-三甲基苄基)丙烯腈(苯胺基物)的制备是TMP发展的一个瓶颈。有文献报导以二甲胺基丙腈、三甲醛、苯胺为原料,DMSO为溶剂,产率较高,但DMSO易分解,不易回收,化工异味大。本研究以DMI溶剂,通过产物的分析检测和结构表征表明得到目标产物,反应过程DMI不易分解,化工异味明显改善;苯胺基物结晶颗粒较大,利于固液分离,易于干燥,收率高出两个百分点。因此,用DMI作为溶剂合成苯胺基物是一条更加清洁环保的工艺路线。

Trimethoprim （TMP） is one of the pillars of our pharmaceutical industry, but the key intermediates aniline - based preparation is a bottleneck in the development of TMP. Literature reported to dimethyl amino propyl cyanide, the three methoxy benzaldehyde, aniline is the three raw materials, DMSO as solvent, high yield, but DMSO can decompose, it is difficult to recycle, chemical odor very big. Studying in DMI solvent, through analysis of detection and characterization shows that the target product, DMI is not easy to break down the response process, chemical odors significantly improved; Aniline - based crystalline particles of larger, conducive to solid - liquid separation, easy to dry, two percentage points higher yield. Therefore, DMI as solvent of synthesis of aniline - based is a cleaner environmentally friendly mute.