摘要
以二甲苯为溶剂,丙二酸二乙酯和苯胺为原料,在物料比为n(丙二酸二乙酯)∶n(苯胺)=1∶2.2的条件下,采用边反应边将乙醇蒸出的方法,回流反应4 h,得到N,N′-二苯基丙二酰胺粗产物,用异丙醇作溶剂,以自行设计改进的缩合双套管分离装置为提取器,将粗产物中的杂质萃取,获得N,N′-二苯基丙二酰胺的质量分数大于98%,收率可达92%。通过熔点I、R谱及元素的测定对产物进行了表征。
N, N＇-Diphenylmalonamide with a purity of 98 % was prepared by reaction of malonic ester and aniline with a molecular ratio of 1 ： 2.2 in xylene. Ethanal was distilled out from the reaction mixture during reaction, and then the mixture was refluxed for 4 h. The extraction was carried out by using isopropanol as extractant and a twin-tube separation instrument designed and made by ourself. The target compound was confirmed by melting poin test, IR spectroscopy and elemental analysis. The yield was 92 % .
出处
《化学世界》
CAS
CSCD
北大核心
2006年第2期102-104,共3页
Chemical World
基金
上海高等学校科学技术发展基金项目(03KH11)
上海市重点学科建设基金项目(P1502)
