有机化学 ›› 2019, Vol. 39 ›› Issue (5): 1323-1332.DOI: 10.6023/cjoc201811021 上一篇    下一篇

研究论文

微波辐射下超细高岭土催化的肟类化合物的高效合成

梁玲, 牟佳玲, 陈悦, 王梦莎, 洪志   

  1. 台州学院医药化工与材料工程学院 台州 318000
  • 收稿日期:2018-11-17 修回日期:2019-02-13 出版日期:2019-05-25 发布日期:2019-03-29
  • 通讯作者: 洪志 E-mail:zhihong@tzc.edu.cn
  • 基金资助:

    浙江省基础公益研究计划(No.LGG18B020002)资助项目.

An Efficient Synthesis of Oxime Compounds Catalyzed by Superfine Kaolin under Microwave Irradiation

Liang Ling, Mou Jialing, Chen Yue, Wang Mengsha, Hong Zhi   

  1. School of Pharmaceutical and Materials Engineering, Taizhou University, Taizhou 318000
  • Received:2018-11-17 Revised:2019-02-13 Online:2019-05-25 Published:2019-03-29
  • Contact: 10.6023/cjoc201811021 E-mail:zhihong@tzc.edu.cn
  • Supported by:

    Project supported by the Basic Public Research Project of Zhejiang Province (No. LGG18B020002).

以廉价易得的超细高岭土为催化剂,羰基类化合物和盐酸羟胺为原料,PEG-400为溶剂,在微波辐射的条件下高效地合成一系列肟类化合物,同时探究了催化剂、溶剂种类、反应时间、反应温度等条件对反应的影响,并对所得的产物进行了熔点、核磁、红外、质谱数据检测.该方法具有反应时间短(5~15 min)、产率高、操作简便和环境友好等优点.另外,也初步探索了超细高岭土催化的微波辐射下肟交换反应及肟醚类化合物合成反应,产率分别为42%~67%与59%~72%.

关键词: 超细高岭土, 微波, 肟类化合物, 催化, 肟交换反应, 肟醚类化合物

Oxime compounds were efficiently synthesized with aromatic or aliphatic ketones and hydroxylamine hydrochloride as raw materials in the PEG-400 solution, using cheap and readily available superfine kaolin as catalyst under microwave irradiation condition. The effects of the catalyst, the solvent type, reaction time, reaction temperature on the reaction were investigated. The structures of the products were detected by melting point, nuclear magnetic resonance, infrared spectroscopy and mass spectrometry data. This method has the advantages of short reaction times (5~15 min), good yields, and simple operation as well as environmental friendliness. In addition, the preliminary experiment shows that superfine kaolin could also catalyze transoximation reaction and preparation of oxime ether compounds under microwave irradiation with the yields of 42%~67% and 59%~72%.

Key words: superfine kaolin, microwave, oxime compound, catalysis, transoximation, oxime ether compounds