SCI和EI收录∣中国化工学会会刊

中国化学工程学报 ›› 2020, Vol. 28 ›› Issue (5): 1320-1325.DOI: 10.1016/j.cjche.2020.02.002

• Catalysis, Kinetics and Reaction Engineering • 上一篇    下一篇

A circular microreaction method to the safe and efficient synthesis of 3-methylpyridine-N-oxide

Funing Sang, Jinpei Huang, Jianhong Xu   

  1. The State Key Lab of Chemical Engineering, Department of Chemical Engineering, Tsinghua University, Beijing 100084, China
  • 收稿日期:2019-12-30 修回日期:2020-01-31 出版日期:2020-05-28 发布日期:2020-07-29
  • 通讯作者: Jianhong Xu
  • 基金资助:
    The authors gratefully acknowledge the supports of the National Natural Science Foundation of China (21991101, 2191100) and the Key Project of Science & Technology Department of Sichuan Province (2017JZ0011) for this work.

A circular microreaction method to the safe and efficient synthesis of 3-methylpyridine-N-oxide

Funing Sang, Jinpei Huang, Jianhong Xu   

  1. The State Key Lab of Chemical Engineering, Department of Chemical Engineering, Tsinghua University, Beijing 100084, China
  • Received:2019-12-30 Revised:2020-01-31 Online:2020-05-28 Published:2020-07-29
  • Contact: Jianhong Xu
  • Supported by:
    The authors gratefully acknowledge the supports of the National Natural Science Foundation of China (21991101, 2191100) and the Key Project of Science & Technology Department of Sichuan Province (2017JZ0011) for this work.

摘要: 3-Methylpyridine-N-oxide is an essential intermediate in the preparation of 2-chloro-5-methylpyridine, which can be used to synthesize nicotine insecticides such as imidacloprid and acetamiprid. The traditional method of production of 3-methylpyridine-N-oxide is catalytic oxidation of 3-methylpyridine in semi-batch reactors. Due to strong exothermic reaction and explosive property of 3-methylpyridine, the reaction efficiency and safety is low using batch technology. Therefore, the development of a safer and efficient 3-methylpyridine-N-oxide production process is very necessary in industrial production. In this paper, microreaction systems were introduced into the preparation of 3-methylpyridine-N-oxide. The comparison of three different methods (traditional semibatch method, co-current microreaction method, and circular microreaction method) showed that the circular microreaction method was the most applicable, with relative higher product yield (~90%), less side reaction and better reaction control.

关键词: Flow synthesis, Hydrogen peroxide, Oxidation, Microreaction system

Abstract: 3-Methylpyridine-N-oxide is an essential intermediate in the preparation of 2-chloro-5-methylpyridine, which can be used to synthesize nicotine insecticides such as imidacloprid and acetamiprid. The traditional method of production of 3-methylpyridine-N-oxide is catalytic oxidation of 3-methylpyridine in semi-batch reactors. Due to strong exothermic reaction and explosive property of 3-methylpyridine, the reaction efficiency and safety is low using batch technology. Therefore, the development of a safer and efficient 3-methylpyridine-N-oxide production process is very necessary in industrial production. In this paper, microreaction systems were introduced into the preparation of 3-methylpyridine-N-oxide. The comparison of three different methods (traditional semibatch method, co-current microreaction method, and circular microreaction method) showed that the circular microreaction method was the most applicable, with relative higher product yield (~90%), less side reaction and better reaction control.

Key words: Flow synthesis, Hydrogen peroxide, Oxidation, Microreaction system