期刊
CHEMICAL ENGINEERING JOURNAL
卷 262, 期 -, 页码 1168-1174出版社
ELSEVIER SCIENCE SA
DOI: 10.1016/j.cej.2014.10.066
关键词
Microflow; Grignard exchange; Gas-liquid reaction; Carbon dioxide; 2,4,5-Trifluorobenzoic acid
资金
- National Natural Science Foundation [21302095]
- Research Fund for the Doctoral Program of Higher Education [20133221120003]
- Jiangsu Provincial NSFC [BK20130924]
- Foundation of Jiangsu Educational Committee of China [13KJB150019, CXZZ13_0449]
- Project of Priority Academic Program Development of Jiangsu Higher Education Institutions (PAPD)
2,4,5-Trifluorobenzoic acid is a valuable synthetic intermediate with important application in pharmaceutical industry and material science. In this paper, we report a facile continuous microflow process for the synthesis of 2,4,5-trifluorobenzoic acid via the generation of an unstable aryl-Grignard reagent followed by its reaction with gaseous CO2. The microflow system is easily assembled by a simple T-micromixer, a commercial available falling film microreactor, tube microreactor and several pumps. The use of a composed T-micromixer and tube microreactor facilitates the Grignard exchange reaction of 2,4,5-trifluorobromobenzene with ethylmagnesium bromide producing 2,4,5-trifluorophenylmagnesium bromide almost in quantitative yield, and the use of the falling film microreactor enables a highly efficient gas-liquid reaction of the resultant Grignard reagent with CO2 under an atmosphere pressure, which ultimately gave the product 2,4,5-trifluorobenzoic acid in high yield with high purity after a simple and extractive workup. The influence of reaction parameters on the two steps in microreactors was discussed. (C) 2014 Elsevier B.V. All rights reserved.
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