3-((E)-2-丁烯酰基)-1,3-噁唑烷-2-酮的合成

Synthesis of 3-((E)-2-butenoyl)-1,3-oxazolidin-2-one

用一种新的方法合成了3-((E)-2-丁烯酰基)-1,3-唑烷-2-酮,先用(E)-2-丁烯酸与二氯亚砜反应合成(E)-2-丁烯酰氯,再由(E)-2-丁烯酸与(E)-2-丁烯酰氯反应合成(E)-2-丁烯酸酐,最后把(E)-2-丁烯酸酐加入到三乙胺,无水LiCl,1,3-唑烷-2-酮的无水四氢呋喃溶液中,在室温下反应5h,正己烷重结晶得3-((E)-2-丁烯酰基)-1,3-唑烷-2-酮,产率80%。并确定了反应的最佳条件反应温度为25℃,反应时间为5h,催化剂无水LiCl与1,3-唑烷-2-酮的摩尔比为1∶1。

A new method was described for the synthesis of 3 - （（E） - 2- Butenoyl） - 1,3 - oxazolidin- 2- one. Crotonic acid reacts with thiony] chloride to produce crotonyl chloride. Crotonyl chloride reacts with erotonic acid to produce crotonic anhydride. Crontonic anhydride was added to anhydrous THF lriethylamine, anhydrous lithium chloride and 1,3 - oxazolidin- 2- one, then stirred at room temperature for 6 hours, crystallize with hexane to abtain production with yield of 80% .The optional reaction conditions were as follows： reaction temperature was .25℃ ;reaction time was 5 hours; the molar ration of anhydrous lithium chloride to1,3 - oxazolidin - 2 - one was 1 ： 1.