SYNTHETIC MODIFICATION AND SCALE-UP PROCESS FOR 1,1-DIAMINO-2,2-DINITROETHENE (FOX-7)

摘要

Many different synthetic routes to FOX-7 have been developed until now. Each starting material such as 2-methylimidazole, 2-methoxy-2-methylimidazolidine-4,5-dione, or 2-methylpyrimidine-4,6-dione (4,6-dihydroxy-2-methylpyrimidine), was nitrated and then hydrolyzed to FOX-7 by somewhat different process, but the yields were more or less low and the processes were felt a little boring. In our modified process from 4,6-dihydroxy-2-methylpyrimidine, FOX-7 was synthesized in about 90 % yield within several hours. The reaction temperature was well controlled in the preparation of 4,6-dihydroxy-2-methylpyrimidine, while some heat was evolved at the beginning of nitration, judging from a reaction calorimeter.