论文部分内容阅读
以溴代丁二酮为原料,分别从加料方式、酸度、原料摩尔比等方面优化了溴甲基取代甘脲的合成工艺。在溴代丁二酮与尿素的摩尔比为1∶5、加入水-乙醇混合溶剂、搅拌24h后加入溶剂体积2.5%的三氟乙酸、反应48h条件下,产率达60.8%。相对文献[10],本法产率提高了20%~30%。并利用溴甲基取代甘脲与多聚甲醛在氢溴酸-冰乙酸体系下75℃恒温反应1h,得溴甲基取代甘脲二醚,产率达65.5%。在利用核磁共振技术对化合物的结构及性能进行检测和表征的同时,使用X射线单晶衍射技术确定了其中两个化合物的晶体结构。
With bromobutanone as raw material, the synthesis of bromomethyl substituted glycoluril was optimized from the aspects of feeding method, acidity, molar ratio of raw materials and so on. The molar ratio of bromobutanone and urea was 1: 5, added water-ethanol mixed solvent, and stirred for 24 h, then added 2.5% of the solvent volume of trifluoroacetic acid. The reaction yield reached 60.8% under 48h reaction conditions. Relative literature [10], the yield increased by 20% to 30%. Bromomethyl-substituted glycoluril was reacted with paraformaldehyde in hydrobromic acid-glacial acetic acid system at 75 ℃ for 1h to obtain bromomethyl substituted glycoluril, yielding 65.5%. The structure and properties of the compounds were detected and characterized by NMR, and the crystal structures of two compounds were determined by X-ray single crystal diffraction.