2-(4′-氨基苯甲酰基)苯甲酸的合成方法改进

Improvement on the Synthesis Method of 2-(4′-aminobenzoyl)benzoic Acid

以邻苯二甲酸酐,乙酰苯胺为原料,二氯乙烷为溶剂,无水三氯化铝为催化剂,通过Friedel-Crafts酰基化反应制得2-(4′-乙酰氨基苯甲酰基)苯甲酸(1),1在酸性条件下回流,除去乙酰基得到2-(4′-氨基苯甲酰基)苯甲酸(2)。通过1H NMR,IR,MS和元素分析对1和2的结构进行了表征。最佳的Friedel-Crafts反应条件为:邻苯二甲酸酐20 mmol,n(邻苯二甲酸酐)∶n(乙酰苯胺)=1∶1,n(邻苯二甲酸酐)∶n(AlCl3)=1∶3,于45℃反应2 h,收率70.4%。

2-（4′-Aeetylaminobenzoyl）benzoic acid（ 1 ） was synthesized by Friedel-Crafts reaction from o-phthalie anhydride and acetanilide using AlCl3 as a catalyst and 1,2-diehlorethene as a solvent. 2 was obtained from 1 in acid solution by removing aeetyl. The structures of 1 and 2 were characterized by 1^H NMR, IR, MS and elemental analysis. The optimal Friedel-Crafts reaction conditions were as follows ： o-phthalie anhydride was 20 mmol ; n （ o-phthalie anhydride ） ： n （acetanilide） was 1：1; n（o-phthalie anhydride） ： n（AlCl3） was 1：3; 45 ℃ for 1.5 h; the yield was 70.4%.