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- Title
Synthesis of 5-fluoro-2-nitrobenzotrifluoride in a continuous-flow millireactor with a safe and efficient protocol.
- Authors
Chen, Peng; Shen, Chong; Qiu, Min; Wu, Jing; Bai, Yingjun; Su, Yuanhai
- Abstract
A synthesis process of 5-fluoro-2-nitrobenzotrifluoride was achieved in a continuous-flow millireactor system through the nitration of 3-fluorobenzotrifluoride using the mixed acid as a nitrating agent. The process safety was evaluated based on the temperature rise with the use of Reaction Calorimeter and Differential Scanning Calorimetry. The mass transfer limitation for this nitration process in the millireactor was evaluated. Effects of the composition of the mixed acid, the molar ratio of nitric acid to the substrate, the residence time, and the temperature on the reaction performance in the millireactor were studied in order to obtain optimal operational conditions. A heat transfer assessment was made to discuss the effects of the residence time and the inner diameter on the temperature distribution and the substrate conversion. Compared with the traditional batch reactor, the flow reactor could achieve better control over impurity and higher process efficiency because of its enhanced mass and heat transfer rates under the optimized conditions. This continuous-flow synthesis strategy would be beneficial for the commercial manufacturing of fine chemicals and pharmaceutical intermediates with the involvement of nitration.
- Subjects
PHARMACEUTICAL chemicals manufacturing; DRUG factories; TEMPERATURE distribution; MASS transfer; DIFFERENTIAL scanning calorimetry; NITRATION
- Publication
Journal of Flow Chemistry, 2020, Vol 10, Issue 1, p207
- ISSN
2062-249X
- Publication type
Article
- DOI
10.1007/s41981-019-00068-3