摘要
探讨了由对溴苯甲醛与盐酸羟胺反应生成对溴苯甲醛肟、再与甲酸发生氰化反应得到对溴苯腈的合成路线,得到最佳工艺参数为:对溴苯甲醛:盐酸羟胺:甲酸=9.25:4.5:55(质量比),肟化反应温度为70-75℃,时间为60min,氰化反应温度为回流温度,时间为1.5h,得到的对溴苯腈纯度大于99%,收率为98.7%。与原有方法相比,本方法采用无水硫酸钠处理含水甲酸,大大降低了成本。
Theoptimumtechnicalparameterforsynthesizing4-bromobenzonitrileisasfollows:theweightratioof4-bromobenzaldehydetoformicacidis2,theweightratioofformicacidtohydroxylaminehydrochlorideis10,thetemperatureandtimeofoximationreactionare70~75℃and60minutesrespectively,thetemperatureandtimeofcyanidationreactionarecircumfluencetemperatureand1.5hoursrespectively.Thepurityof4-bromobenzonitrileisabove99%andtheyieldis98.7%.Comparedwithothermethods,thissynthesisreducedcostconsumedlyinthatsodiumsulfateisusedtoprocessformicacidcontainingwater.Moreoverthesynthesisof4-bromobenzaldehydewasresearchedandthetechnicalparametersapttoindustrialmanufacturewereacquired.
出处
《茂名学院学报》
2005年第1期19-22,共4页
Journal of Maoming College
关键词
对溴苯腈
对溴苯甲醛
氰化
4-bromobenzaldehyde
4-bromobenzonitrile
cyanidation