摘要
在盐酸存在下,以对氨基苯甲酸和双氰胺为基本原料,一步合成了对双胍基苯甲酸盐酸盐(CPBGH),通过正交实验方法优化了合成条件,用FT IR、1H NMR和UV表征了产物结构,HPLC分析了产品中CPBGH的含量。结果表明,CPBGH适宜的合成条件为:盐酸与对氨基苯甲酸摩尔比为1.0,反应温度为80℃,反应时间为6.0 h;在此条件下,CPBGH的收率为86.1%。UV分析表明,CPBGH在191 nm、237 nm和269 nm有三个明显的紫外吸收峰;HPLC分析表明,产品中CPBGH的含量达97.22%。
One pot method was utilized to synthesize 1-(p-carboxyphenyl) biguanide hydrochloride(CPBGH) with p-aminobenzoic acid(PABA) and dicyandiamide(DCDA) as starting material in the presence of hydrochloric acid.The synthetic conditions were optimized according to orthogonal experiment results.The structure of product was characterized by FT IR,()~1H NMR and UV and the content of CPBGH in the product was determined by HPLC.Experimental results indicated that the suitable conditions for the synthesis of CPBGH were as follows:the molar ratio of hydrochloric acid to p-aminobenzoic acid was 1.0,the reaction temperature was 80℃ and the reaction time was 6.0 h.Under these conditions,the yield of product was about 86.1%.Result of UV analysis showed there were three adsorbing peaks at 191 nm,237 nm and 269 nm,respectively.Result of HPLC analysis indicated the content of CPBGH in the product was up to 97.22%.
出处
《化学世界》
CAS
CSCD
北大核心
2010年第4期232-234,242,共4页
Chemical World
基金
江苏省应用化学重点学科及建设开放基金项目(XKY2009005)
关键词
对双胍基苯甲酸盐酸盐
条件优化
正交实验
1-(p-carboxyphenyl) biguanide hydrochloride
optimization of conditions
orthogonal experiment