微波促进卤素交换氟化反应合成邻氟苯腈的研究

刘建武, 严生虎, 张跃

现代化工 ›› 2021, Vol. 41 ›› Issue (5) : 148 -152.

PDF (1499KB)
现代化工 ›› 2021, Vol. 41 ›› Issue (5) : 148-152. DOI: 10.16606/j.cnki.issn0253-4320.2021.05.030
科研与开发

微波促进卤素交换氟化反应合成邻氟苯腈的研究

    刘建武, 严生虎, 张跃
作者信息 +

Synthesis of o-fluorobenzonitrile by microwave-assisted halogen exchange fluorination

Author information +
文章历史 +
PDF (1534K)

摘要

以邻氯苯腈(OCBN)和氟化钾为原料、N,N-二甲基丙烯基脲(DMPU)为溶剂、四苯基溴化膦为相转移催化剂,在微波反应器中通过卤素交换氟化合成邻氟苯腈(OFBN)。考察了加热方式、溶剂及其用量、催化剂、物料摩尔比、温度和时间等对氟化反应的影响,得到的最佳工艺条件为:n(邻氯苯腈):n(KF)=1:3、溶剂V(DMPU)=20 mL、微波功率P=300 W、反应温度为210℃、反应时间为4 h,此时邻氯苯腈转化率达85.8%,邻氟苯腈收率达71.5%。与常规加热相比,微波辐射可以加快卤素交换氟化反应速率,提高产品收率。

Abstract

o-Fluorobenzonitrile (OFBN) is prepared through halogen exchange fluorination in a microwave reactor,using o-chlorobenzonitrile (OCBN) and KF as raw materials,N,N-dimethylpropenylurea (DMPU) as solvent and tetraphenylphosphonium bromide as phase transfer catalyst.The Influencing factors on fluorination are investigated,including heating method,solvent types,solvent dosage,catalyst,materials ratio,temperature and time.The optimum reaction conditions are obtained as follows:n(o-chlorobenzonitrile):n(KF)=1:3,solvent V(DMPU)=20 mL,microwave power P=300 W,temperature at 210℃,and reaction time for 4 h.Under the optimal conditions,the conversion of o-chlorobenzonitrile reaches 85.8%,and the yield of o-fluorobenzonitrile reaches 71.5%.Compared with conventional heating method,microwave irradiation can accelerate the reaction speed of halogen exchange fluorination and improve the yield of product.

关键词

微波 / 相转移催化剂 / 卤素交换 / 邻氟苯腈

Key words

microwave / phase transfer catalyst / halogen exchange / o-fluorobenzonitrile

引用本文

引用格式 ▾
微波促进卤素交换氟化反应合成邻氟苯腈的研究[J]. 现代化工, 2021, 41(5): 148-152 DOI:10.16606/j.cnki.issn0253-4320.2021.05.030

登录浏览全文

4963

注册一个新账户 忘记密码

参考文献

AI Summary AI Mindmap
PDF (1499KB)

290

访问

0

被引

导航
相关文章

AI思维导图

/