对双胍基苯甲酸盐酸盐的制备及其合成条件优化.pdf

化学世界
2010年
对双胍基苯甲酸盐酸盐的制备及其合成条件优化
金绍娣2,姚成2,蔡照胜
(1盐城工学院化学与生物工程学院,江苏盐城224003;2.南京工业大学理学院,江苏南京210009)
摘要:在盐酸存在下,以对基苯甲酸和双氰胺为基本原料,一步合成了对双豚基苯甲酸盐酸盐
( CPBGE),通过正交实验方法优化了合成条件,用FTIR、HNMR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:盐酸与对基苯甲
酸摩尔比为1.0,反应湿度为80℃,反应时间为6.0h;在此条件下, CPBGH的收率为86.1%。UV
分析表明, CPBGE在191nm、237nm和269nm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%。
关键词:对双胍基苯甲酸盐酸盐;条件优化;正交实验
中图分类号:O622
文献标志码:A
文章编号:0367-6358(2010)04-0232-04
Preparation of 1-(2-carboxyphenyl) biguanide Hydrochloride
and Optimization of the Synthetic Conditions
JIN Shao-dil2, YAO Cheng, CAI Zhao-sheng
(1. School of Chemical and Biological Engineering, Yancheng Institute of Technology, Jiangsu Yancheng 224003, China
2. School of Science, Naniing University of Technology, Jiangsu Naniing 210009, China)
Abstract: 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, H 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 80C 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%
Key words: 1-(2-carboxyphenyl biguanide hydrochloride; optimization of conditions; orthogonal
experiment
双胍类化合物可通过胍基与生物体中的某些特谢发生改变,从而显示很高的抗菌和杀菌等生物活
定基团或元素作用,使生物体正常的物质和能量代性。双胍类化合物作为广谱杀菌剂已经得到广泛应
收稿日期:2009-08-25
甚金项目:江苏省应用化学重点学科及建设开放基金项目(XKY2009005)
作者简介:金绍娣(1983~),女,江苏扬州人,硕士生,主要从事糟细有机合成以及精细化学品的开发研究工作。 E-mail: jinshaodi(
163. com *e-mail: jsc. czs@163. com