氯代邻羟基二苯醚类化合物的合成工艺  

Synthesis and Technics of Chloro-o-Hydroxyldroxyl Ethers

作　　者：卢俊瑞[1] 辛春伟[2] 尹宁[2] 陈丽然[2] 马霞苗[2] 刘芳[2] 张明[2] 

机构地区：[1]天津大学药物科学与技术学院,天津300072 [2]天津理工大学化学化工学院,天津300191

出　　处：《天津大学学报》2008年第6期714-719,共6页Journal of Tianjin University(Science and Technology)

基　　金：国家自然科学基金资助项目(20576103,20776114);天津市自然科学基金资助项目(05YFJIYJC14000)

摘　　要：氯代邻羟基二苯醚类化合物被广泛用作杀菌剂、医药及日化、卫生用品等的抗菌成分.目前,该类化合物主要通过氯代邻氨基二苯醚重氮化水解反应制得,由于制备过程伴有分子内关环副反应,导致产品收率和质量很低.文中对影响氯代邻氨基二苯醚重氮化水解反应的主要因素和工艺条件进行了系统研究,结果表明,取代基对氯代邻氨基二苯醚重氮盐的水解和分子内关环反应的选择性有重要影响,金属离子对分子内关环反应有显著催化作用,制备氯代邻羟基二苯醚的较佳工艺条件为:重氮化硫酸质量分数为95%～98%;水解硫酸质量分数为74%～78%;重氮化温度为55～60℃;水解温度为160～175℃.Chloro-o-hydroxyldiphenyl ethers, as antimicrobial, are widely used in the fields of disinfectant, medicine and health care. These compounds are prepared through hydrolyzing the diazo salt of chloro-o-arninodiphenyl ethers at present. Because the hydrolization is accompanied with the side reaction of intra molecular cyclization, the yield and quality of the title products are low. The factors and the processing conditions for hydrolyzing chloro-o-aminodiphenyl ethers were studied. The results show that the substituted groups have great influence on selection of the hydrolyzation and the intra molecular cyclization; the metal cations observably catalyze the intra molecular cyclization of chloro-o-amiodipheyl diazaonium salts ; the optimum preparation conditions of the title products are that, the concentrations of sulfuric acid used to diazotize and hydrolyze are 95%--98% and 74%--78%, respectively, and the temperature of diazotization and hydrolyzation is 55-- 60℃ and 160--175℃,respectively.

关 键 词：氯代邻羟基二苯醚 抗菌剂 合成 工艺条件 

分 类 号：TQ243.2[化学工程—有机化工]