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