doi:10.16597/j.cnki.issn.1002-154x.2023.01.004
对肼基苯磺酸的合成工艺研究
姬金岭 樊平平 赵慧 石佳 王运良∗
(佳木斯大学 药学院, 黑龙江 佳木斯 154007)
Study on the Synthesis Process of p-Hydrazinobenzenesulfonic Acid
Ji Jinling; Fan Pingping; Zhao Hui; Shi Jia; Wang Yunliang ∗;
(College of pharmacy, Jiamusi University, Heilongjiang Jiamusi 154007)
摘要:
作者对对肼基苯磺酸合成路线进行了优化。 以对氨基苯磺酸为原料,经过重氮化反应和还原反应,一锅法合 成对肼基苯磺酸。 选取碱种类、浓盐酸的用量、反应温度 3 个因素,利用正交实验对反应进行优化,得到最佳反应条件为 2 g 对氨基苯磺酸用 11.5 mL 5% 氢氧化钠溶液溶解,再用 8.0 mL 浓盐酸进行重氮化,之后再还原反应即可得产品,平均收率为 75.0% 。 对优化后的工艺进行中试放大试验,反应条件温和,操作简便,收率稳定,具有一定的工业化应用前景。
关键词：对肼基苯磺酸；对氨基苯磺酸；重氮化反应；合成；
Abstract：
The synthesis route of p-hydrazinobenzenesulfonic acid was optimized. Using p-aminobenzenesulfonic acid as raw material, p-hydrazinobenzenesulfonic acid was synthesized by diazotization reaction and reduction reaction in one pot. The reaction was optimized by orthogonal test with three factors including the type of alkali, the amount of concentrated hydrochloric acid and the reaction temperature. The optimal reaction conditions were obtained as follows: 2 g p-aminobenzene sulfonic acid was dissolved in 11.5 mL 5% sodium hydroxide solution, and then was diazotized with 8.0 mL concentrated hydrochloric acid, and then was reduced at 100 ℃ . The average yield was 75% . The pilotscale test of the optimized process showed that the reaction conditions were mild, the operation was simple, the yield was stable, and it had a certain industrial application prospect.
Keywords：p-hydrazinobenzenesulfonic acid; p-aminobenzenesulfonic acid; diazotization reaction; synthesis;