摘要
以邻氯苯甲酸为原料,采用混酸硝化生成中间体2-氯-5-硝基苯甲酸,再水解生成目标产物5-硝基水杨酸.重点对硝化反应的混酸配比、反应温度及水解反应的反应温度、反应时间进行了考察,得到了硝化反应混酸配比为浓硫酸∶浓硝酸(摩尔比)=9∶1,反应温度0℃,反应时间为8h的较优工艺条件,收率为95.7%.水解反应温度为140℃,反应时间为16h,收率为98.3%.反应后产品用适量乙醇水溶液重结晶得到5-硝基水杨酸,含量≥99.8%(HPLC).
The process of synthesizing 5-nitrosalicylic acid by nitration and hydrolysis of o-chlorobenzoic acid was developed and investigated. The influences of the nitration of temperature, proportion of mixed acid and of the hydrolysis of temperature, reaction time were investigated. The yield of nitration was 95.7% with a mixed acid of nitric acid∶sulfuric acid=9∶1, in the course of 0 ℃ and 8h, and the yield of hydrolysis was 98.3% in the course of 140 ℃ and 16 h. The final product (HPLC≥99.8%) was obtained after recrystallizing by the proper ethanol solution.
出处
《浙江工业大学学报》
CAS
2005年第1期96-99,共4页
Journal of Zhejiang University of Technology
