摘要
以放大生产为目的研究了1,3,5-三(3-溴苯基)苯的合成工艺,探讨了投料比、反应温度、反应时间对产品收率的影响,推断出了可能的反应机理.结果表明,合成1,3,5-三(3-溴苯基)苯的最佳反应条件是:n(间溴苯乙酮)∶n(氯化亚砜)=1∶1.6,反应温度为78℃,反应时间为4 h.按照此反应条件逐步放大到千克级,平行三批实验的平均收率为90.6%,平均含量为98.3%.
The synthetic routes of 1,3,5-tris(3-bromophenyl)benzene are reviewed,and synthetic process of 1,3,5-tris(3-bromophenyl)benzene studied for scale-up production.The effect of feed ratio,reaction temperature and time on product yield are discussed,and possible reaction mechanism is deduced.Results show that the best reaction conditions for synthesizing 1,3,5-tris(3-bromophenyl)benzene are:n(m-bromoacetophenone)∶n(sulfoxide)=1∶1.6,reaction temperature is 78℃and reaction time 4 h.It is gradually scaled up to the kilogram level.The average yield of three parallel experiments is 90.6%,and average content 98.3%.
作者
赵立献
王凤伟
王翠丽
ZHAO Li-xian;WANG Feng-wei;WANG Cui-li(Department of Research and Development,Shijiazhuang Jiuda Technology Co.,Ltd.,Shijiazhuang,Hebei 051434,China)
出处
《石家庄职业技术学院学报》
2019年第6期28-31,共4页
Journal of Shijiazhuang College of Applied Technology
作者简介
赵立献(1982-),男,石家庄九达科技有限公司工程师,硕士,研究方向:有机合成研究及放大生产.