摘要
研究以甲酸和苯胺为原料,催化脱水合成N,N’-二苯基甲脒的工艺条件。采用单因素试验对影响因素进行探讨。得到最佳制备工艺条件为:甲酸4.6 g(0.1 mol),苯胺32.55 g(0.35 mol),脱水剂二甲苯30 mL,催化剂硼砂0.3 g、铁粉1 g,在150℃回流反应6 h。此条件下,产品最高收率可达91.5%。该工艺原料廉价易得,操作简便安全,收率高,适合工业化大生产。
To explore the optimal condition for synthetising N,N'-diphenylformamidine from formic acid and aniline by catalyzed dehydration,the factors for effecting synthesis process were discussed by single factor tests.It is resulted that best conditions was showed as follows:using 30 mL dimethylbenzene as dehydrator,formic acid 4.6 g(0.1 mol),aniline 32.55 g(0.35 mol),cast iron 1 g,borax 0.3 g,reaction temperature 150 ℃,reaction time 6 h.The total yield was 91.5 %,The structures were characterized by 1H NMR and 13C NMR spectra.It is conclused that synthetic process is advantages of high yield,simple operation and safety and is possible of industrialized production.
出处
《科学技术与工程》
北大核心
2012年第5期1185-1187,共3页
Science Technology and Engineering
基金
榆林学院高层次人才科研启动基金项目(08GK30)资助
关键词
N
N’-二苯基甲脒
甲酸
苯胺
合成
N
N'-diphenylformamidine formic acid aniline synthesis