一釜合成5-氯水杨酰胺的研究

在一个反应器内,5-氯水杨酸与氯化亚砜反应生成5-氯水杨酰氯,与甲醇反应生成5-氯水杨酸甲酯,再与氨气反应生成5-氯水杨酰胺。中间体不经分离提纯,总收率可达79%。结果表明,最佳氨解反应条件:氨∶5-氯水杨酸甲酯=12∶1(摩尔比),溶剂为甲醇,最佳反应温度为35~40℃,反应时间为15 h。通过IR、MS、NMR光谱分析和元素分析,对产物的结构进行了表征。HPLC测定其纯度为99.54%。

Study on ''''one pot'''' synthesis of 5-chlorosalicylamide

In the presence of methanol,5-chlorosalicyloyl chloride is synthesized from 5-chlorosalicylic acid with thionyl chloride,then 5-chlorosalicyl methyl ester is synthesized by the reaction of 5-chlorosalicyloyl chloride with methanol,finally,5-chlorosalicylamide is synthesized by the reaction of 5-chlorosalicyl methyl ester with ammonia.All the reactions were carried out in one pot.The intermediates do not need separation and purification,the total yield reaches 79%.The result showed the best ammonolysis condition:the ratio of ammonia to 5-chlorosalicyl methyl ester is 12 ∶1,the solvent is methanol,the temperature is 35～40 ℃,the ammonolysis time is 15 h.The structure of the 5-chlorosalicylamide was confirmed by the spectrograms of IR,MS,NMR and elemental analysis.The purity of 5-chlorosalicylamide reaches 99.54%(HPLC).