Balz-Schieman法合成4-氟邻苯二甲酰亚胺

Synthesis of 4-fluorophthalimide by Balz-Schieman

摘要:

4-氟邻苯二甲酰亚胺在国内尚无工业生产，价格昂贵，是合成含氟酞菁化合物的重要中间体。本文主要介绍以4-硝基邻苯二甲酰亚胺为原料，通过Balz-Schieman法制备4-氟邻苯二甲酰亚胺的反应，考察了Balz-Schieman反应中氟硼酸用量对氟硼酸重氮盐收率的影响，得到n（4-氨基邻苯二甲酰亚胺）：n（氟硼酸）=1：4时收率最高，为89.23％。并考察了反应条件对重氮盐加热分解反应的影响，得到最优反应条件：采用液相加热分解方式，氟化钾催化剂存在下，n（原料）：n（氟化钾）=1：2，在130℃分批次投料，反应3小时，4-氟邻苯二甲酰亚胺的收率为43.35％。与以4-氟邻苯二甲酸酐为原料合成4-氟邻苯二甲酰亚胺的方法相比，大大降低了成本，具有工业化的发展前景。

Abstract:

4-fluorophthalimide is an important intermediate for fluorophthalocyanines, but it has not been large-scale commercial produced and the price is high. 4-fluorophthalimide was synthesized with 4-nitrophthalimide by Balz-Schieman method in this paper. The relationship between yield of the diazotization and fluoroboric acid was investigated and the yield could reach 89.23%. The effect of reaction conditions, such as reaction mode, feeding mode, catalyst, reaction time and temperature, on the yield of the thermal decomposition were also investigated and the yield could reach 43.35％. Compared with the way using 4-fluorophthalic anhydride as raw materials, the method reported in this paper reduced cost a lot and is applicable for industrial production.