用于合成 4-硝基吡唑的全连续流工艺

IF 2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Journal of Flow Chemistry Pub Date : 2024-01-31 DOI:10.1007/s41981-024-00311-6
Jiadi Zhou, Zhaoyang Mu, Lishan Geng, Xuyang Zhao, Chenwei Gao, Zhiqun Yu
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引用次数: 0

摘要

4-nitropyrazole 的制备引入了完全连续流硝化和后处理方案。该工艺从吡唑与混合酸的硝化反应开始,然后是连续淬火、中和、萃取和分离。收集的有机相经旋转蒸发回收溶剂后,得到最终产品 4-硝基吡唑,收率 96.9%,纯度 99.3%,生产率 381 g/h。通过建立动力学模型和 MATLAB 仿真计算,实现了单硝化产物 4-硝基吡唑的最佳选择性条件。后处理工艺解决了固体沉淀和萃取剂水解的问题。萃取工艺由分配系数决定,并采用两次萃取以减少有机溶剂用量。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

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A fully continuous-flow process for the synthesis of 4-nitropyrazole

A fully continuous-flow nitration and post-processing protocol has been introduced into the preparation of 4-nitropyrazole. The process started from the nitration reaction of pyrazole with mixed acid, followed by continuous quenching, neutralization, extraction and separation. After the collected organic phase was rotationally evaporated to recover the solvent, the final product 4-nitropyrazole was obtained with 96.9% yield, 99.3% purity and 381 g/h productivity. By establishing a kinetics model and MATLAB simulation calculation, it worked out to achieve the preferable selectivity conditions of mono-nitration product 4-nitropyrazole. The process of post-processing solved the problems of solid precipitation and extractant hydrolysis. The extraction process was determined by the distribution coefficient and twice extraction was used to reduce the amount of organic solvent.

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来源期刊
Journal of Flow Chemistry
Journal of Flow Chemistry CHEMISTRY, MULTIDISCIPLINARY-
CiteScore
6.40
自引率
3.70%
发文量
29
审稿时长
>12 weeks
期刊介绍: The main focus of the journal is flow chemistry in inorganic, organic, analytical and process chemistry in the academic research as well as in applied research and development in the pharmaceutical, agrochemical, fine-chemical, petro- chemical, fragrance industry.
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