Kilogram-Scale Synthesis of 2,4-Dichloro-5-fluorobenzoic Acid by Air Oxidation under the Continuous-Flow Process,Organic Process Research & Development

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Kilogram-Scale Synthesis of 2,4-Dichloro-5-fluorobenzoic Acid by Air Oxidation under the Continuous-Flow Process
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2018-01-23 00:00:00 , DOI: 10.1021/acs.oprd.7b00358
Shaozheng Guo ₁ , Zhiqun Yu ₁ , Chuanming Yu ₁

Affiliation

A continuous-flow process for the preparation of 2,4-dichloro-5-fluorobenzoic acid (BA) has been reported. We chose 2,4-dichloro-5-fluoroacetophenone (AP) as starting material and acetic acid as cosolvent to achieve the excellent results in the continuous-flow oxidization system. The nitric acid oxidation of BA is a violent exothermic reaction. However, the continuous-flow system includes advantages such as good mass and heat transfer to ensure the safety of the reaction. The influences of different factors, including reactant ratio, temperature, and residence time, were investigated based on single factor tests. The optimal reaction conditions were obtained, in which the yield reached up to 100%. Compared with the traditional tank reactor process, less nitric acid consumption, a higher product yield, less reacting time, being more environmental friendly, and process continuity ensuring higher operation safety are achieved in the continuous-flow system.

中文翻译：

连续流空气氧化氧化公斤级合成2,4-二氯-5-氟苯甲酸

已经报道了用于制备2，4-二氯-5-氟苯甲酸（BA）的连续流方法。我们选择了2,4-二氯-5-氟苯乙酮（AP）作为起始原料，并选择乙酸作为助溶剂，以在连续流氧化系统中获得优异的结果。BA的硝酸氧化是剧烈的放热反应。然而，连续流系统包括诸如良好的质量和热传递的优点，以确保反应的安全性。在单因素试验的基础上，研究了反应物比，温度和停留时间等不同因素的影响。获得了最佳反应条件，其中收率达到100％。与传统的槽式反应器工艺相比，在连续流系统中，硝酸消耗更少，产物收率更高，反应时间更少，对环境更友好，过程连续性确保了更高的操作安全性。

更新日期：2018-01-23

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