间苯三酚的合成及工艺优化  

Study on the synthesis process of phloroglucinol

作　　者：刘晓莲 Liu Xiaolian(Hebei Jiheng Pharmaceutical Corporation Ltd.,Hengshui 053400,China)

机构地区：[1]河北冀衡药业股份有限公司,河北衡水053400

出　　处：《煤炭与化工》2024年第2期139-142,共4页Coal and Chemical Industry

基　　金：河北省省级科技计划资助(199676234H)。

摘　　要：提供了一种原料药间苯三酚的合成方法,以2,6-二氯苯酚为合成间苯三酚的起始原料,以高沸点隋性溶剂1,2,4-三甲基苯为分散剂,在氯化亚铜的催化剂作用下,与氢氧化钾在常压下加热搅拌进行消去反应,反应结束加入纯化水进行加成反应,随后静止分层,分出上层溶剂,下层水相用浓盐酸调节pH值2.0至有晶体析出,抽滤干燥得间苯三酚粗品,水相重结晶即得类白色间苯三酚成品。整个工艺过程收率达70%以上,纯度高达99.83%,该合成工艺路线简单,后处理方便易操作,适合工业化生产。A synthesis method for the raw material drug phloroglucinol was provided by using 2,6-dichlorophenol as the starting material and high boiling point solvent 1,2,4-trimethylbenzene as the dispersant.Under the catalysis of cuprous chloride,it reacts with potassium hydroxide under atmospheric pressure and heat stirring to eliminate the reaction.At the end of the reaction,purified water was added for static stratification,and the upper solvent was separated,the pH value of the lower aqueous phase with concentrated hydrochloric acid was adjusted to 2.0 until crystals precipitate,filter and dry the crude product of phloroglucinol,and recrystallize the aqueous phase to obtain a white like product of phloroglucinol.The yield of the entire process is over 70%,and the purity is as high as 99.83%.The synthesis process route is simple,and the post-treatment is convenient and easy to operate,making it suitable for industrial production.

关 键 词：间苯三酚 2 6-二氯苯酚 合成工艺 消去反应 加成反应 

分 类 号：TQ4633[化学工程—制药化工]