Balz-Schieman法合成4-氟邻苯二甲酰亚胺

Synthesis of 4-Fluorophthalimide by Balz-Schieman

以4-硝基邻苯二甲酰亚胺为原料,通过Balz-Schieman法制备了4-氟邻苯二甲酰亚胺,考察了BalzSchieman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89.2%。并考察了反应条件对重氮盐加热分解反应的影响,得到最优反应条件为: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 h,4-氟邻苯二甲酰亚胺的收率为43.4%。

4-Fluorophthalimide was synthesized from 4-nitrophthalimide by Balz-Schieman method. The relationship between the yield of diazotization and the dosage of fluoroboric acid was investigated and the yield could reach 89.2% when n （4-nitrophthalimide） ： n （ fluoroboric acid） was 1：4. 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 43.4%. Compared with the method in which 4-fluorophthalic anhydride is used as raw materials, the raw materials in this paper are easy to get and the reaction conditions are relatively mild.