BITE-101的制备放大工艺研究

The inherent contradiction between the energy and safety of energetic compounds makes the design and synthesis of novel energetic compounds with high density, high energy, strong thermal stability, and high sensitivity characteristics a significant and big challenge. Recently, 4-amino-7,8-dinitropyrazole-[5,1-d][1,2,3,5]-tetrazine-2-oxide (BITE-101), which was characterized to possess superior integrated properties over traditional explosive HMX, was reported by our group. To promote its further applications, the optimized and scale-up preparation of BITE-101 was accomplished in this study, and the effects of acids, the ratio of hydrogen peroxide to acids, and reaction temperature in the oxidation reaction were studied and discussed. The following oxidation conditions were found to be optimal, as follows: compound 1 (60 g, 0.26 mol), concentrated sulfuric acid (120 mL) and H₂O₂ (360 mL). The reaction temperature was 50°C, and a yield of 28.9% was obtained. The BITE-101 preparation procedure was scaled up to 15 g. This study serves as a reference for further research on the application of BITE-101.