摘要
以间二氯苯为原料,经硝化、氟代及还原反应合成2,4-二氟苯胺。探索了各步反应的工艺条件,对提高收率难度较大的氟代反应,研究了使用季铵盐类相转移催化剂时原料配比、反应温度及时间与收率之间的关系,并得到了较好的结果。硝化反应收率达97%,氟代70%,还原89%。与其它方法相比,产品总收率由22%~50%提高到60%以上,从而使文题所示的合成路线成为技术、经济上可行的方法。
Difiuoroaniline was synthesised from l,3 dichlorobenzene as a starting material via nitration,fluorination and reduction,The suitable technological conditions were probed for each step of the reactions.Because it seemed hard to obtain high yields of the fluorination replacement reaction,the relations of the proportions of the raw materials,the reaction temperature and the reaction time to the yields were researched in the presence of a solid liquid phase transfer catalyst using orthogonal design method,Better results have been achieved in experiment.The yield of the nitration reaction was 97%,fluorination 70% and reduction 89%.As compared with the other methods of preparing 2,4-difluoroaniline,the overall yield has been increased from 22%~ 50% to 60% or more.Thus the topical method witch is feasible techno-economically proves the efficient one of preparing 2,4-difluoroaniline.
出处
《华东理工大学学报(自然科学版)》
CAS
CSCD
1996年第3期255-259,共5页
Journal of East China University of Science and Technology
关键词
二氟苯胺
有机合成
还原
间二氯苯
合成
difluoroaniline
organic synthesis
nitration
fluorination
reduction