Chin. J. Org. Chem. ›› 2012, Vol. 32 ›› Issue (01): 165-168.DOI: 10.6023/cjoc1106091 Previous Articles     Next Articles



李清霞, 王鹏, 娄忠良, 刘越, 孟子晖, 徐志斌, 薛敏   

  1. 北京理工大学化工与环境学院 北京 100081
  • 收稿日期:2011-06-09 修回日期:2011-09-02 发布日期:2011-09-23
  • 通讯作者: 孟子晖
  • 基金资助:

    爆炸科学与技术国家重点实验室基金(No. KFJJ09-04)资助项目.

Separation of Key Intermediates in the Synthesis of 1,3,5,7-Tetranitro-1,3,5,7-tetrazocine by Semi-preparative High Performance Liquid Chromatography

Li Qingxia, Wang Peng, Lou Zhongliang, Liu Yue, Meng Zihui, Xu Zhibing, Xue Min   

  1. School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing 100081
  • Received:2011-06-09 Revised:2011-09-02 Published:2011-09-23
  • Contact: Zihui Meng
  • Supported by:

    Project supported by the State Key Laboratory of Explosion Science and Technology (No. KFJJ09-04).

1,3,5,7-Tetraacetyl-1,3,5,7-tetraazacyclooctane (TAT) was a key intermediates for the synthesis of 1,3,5,7-tetranitro- 1,3,5,7-tetrazocine (HMX) that is a highly energetic material. TAT can be prepared from the acetylation of 3,7-diacetyl- 1,3,5,7-tetraazacyclooctane (DAPT) and the small molecules condensation reaction. In this paper, sem preparative high performance piquid chromatography (SPHPLC) was used as a new separation and purification method for the intermediates in the reaction solution, and six samples obtained with high purity (>97%) analyzed by HPLC could prove much evidence and information for the reaction mechanism research. The optimum technological parameters of SPHPLC as follows: Si column (20 mm×250 mm, 10~20 μm), V(acetonitrile)∶V(water)=95∶5 (for the method of the acetylation of DAPT), V(acetonitrile)∶ V(methanol)=90∶10 (for the method of the small molecules condensation reaction), 10 mL·min-1, 215 nm, 1 mL (30 mg· mL-1).

Key words: 1,3,5,7-tetraacetyl-1,3,5,7-tetraazacyclooctane, sem preparative high performance liquid chromatography, HMX, reaction mechanism