3,5-二叔丁基-4-羟基苯甲酸的合成  

Synthesis of 3,5-di-tert-butyl-4-hydroxybenzoic acid

作　　者：张天宇 严宁宁 李效军[1] Zhang Tianyu;Yan Ningning;Li Xiaojun(Department of Chemical Engineering,Hebei University of Technology,Tianjin 300130,China)

机构地区：[1]河北工业大学化工学院

出　　处：《石油化工》2019年第11期1105-1109,共5页Petrochemical Technology

摘　　要：以2,6-二叔丁基苯酚为原料、四氯化碳为烷基化试剂合成了3,5-二叔丁基-4-羟基苯甲酸,利用1HNMR对合成的3,5-二叔丁基-4-羟基苯甲酸进行表征,通过单因素实验和正交实验确定了最佳反应条件。实验结果表明,以四氯化碳为烷基化试剂可实现3,5-二叔丁基-4-羟基苯甲酸的合成,当采用将酸滴加至滤液中时,在n(2,6-二叔丁基苯酚)∶n(四氯化碳)=1∶1.3、烷基化时间为2 h、烷基化温度为70℃、水解时间为6 h条件下,3,5-二叔丁基-4-羟基苯甲酸的收率为93.0%,纯度可达99.3%(w)。3,5-di-tert-butyl-4-hydroxybenzoic acid was synthesized with 2,6-di-tert-butylphenol as raw materials and carbon tetrachloride as alkylating agent. The 3,5-di-tert-butyl-4-hydroxybenzoic acid was characterized by 1 H NMR. The optimal conditions in the reaction were determined by single factor experiments and orthogonal experiments. The experiment results showed that the 3,5-di-tert-butyl-4-hydroxybenzoic acid can be synthesized successfully by using carbon tetrachloride as alkylating agent. When the acid was dropped in the filtrate,n(2,6-di-tert-butylphenol)∶n(carbon tetrachloride)=1∶1.3,the alkylation time was 2 h,the alkylation temperature was 70 ℃,and the hydrolysis time was 6 h. Under these conditions,the yield of 3,5-di-tert-butyl-4-hydroxybenzoic acid is 93.0%,and the purity reaches 99.3%(w).

关 键 词：3 5-二叔丁基-4-羟基苯甲酸 2 6-二叔丁基苯酚 四氯化碳 合成 

分 类 号：TQ047.4[化学工程]