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

作者：Yu, Zhiqun; Lv, Yanwen; Yu, Chuanming^*

来源：Organic Process Research & Development, 2012, 16(10): 1669-1672.

DOI：10.1021/op300127x

• CHEMISTRY
• GENERATION
• REACTORS

An expeditious and multikilogram-scale process for the Balz-Schiemann 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 degrees 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.

• 出版日期2012-10
• 单位衢州学院; 浙江工业大学