A Continuous Kilogram-Scale Process for the Manufacture of o-Difluorobenzene

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• 作者：Zhiqun Yu ; Yanwen Lv ; Chuanming Yu
• 刊名：Organic Process Research & Development
• 出版年：2012
• 出版时间：October 19, 2012
• 年：2012
• 卷：16
• 期：10
• 页码：1669-1672
• 全文大小：229K
• 年卷期：v.16,no.10(October 19, 2012)
• ISSN：1520-586X

文摘

An expeditious and multikilogram-scale process for the Balz鈥揝chiemann synthesis of o-difluorobenzene from o-fluoroaniline via two separate continuous flow reactors in 90.0% yield has been set up. The main steps involved the generation of stable diazonium fluoborate intermediate in situ via continuous diazotization reactor at 20 掳C, and the choice of o-difluorobenzene as cosolvent to achieve the continuous flow fluorodediazoniation system. Reaction time of both steps could be brought down to within 10 s and 2 min, respectively, by increasing the reaction temperature and thereby taking advantage of improved mass and heat transfer of a continuous flow system.