One-pot Method for Synthesis of 1,1-Diamino-2,2-nitroethylene to Improve Process Safety

摘要

1,1-Diamino-2,2-dinitroethylene(DADNE, FOX-7) is a new insensitive explosive.The synthesis processing is relatively complex in literature methods.In literature methods, the intermediate compound must be isolated, and the intermediate compound is very sensitive to mechanical stimuli.The aim of this paper is to explore one-pot method for synthesis of 1,1-Diamino-2,2-nitroethylene to improve process safety.The nitration agent was continuously added into the mixture of 2-methyl-4,6-dthydroxypyrimidine and dichloromethane solvent by peristaltic pump at room temperature.Then water was continuously added into the reaction system to complete the hydrolysis reaction.At last, the solid product FOX-7 was obtained through filtering, washing and drying.The yield of FOX-7 was up to 82.6％ and the purity was 98.0％.By adding an inert solvent to disperse reactants, reaction was milder and the increase of system temperature was less than 5 °C.This synthesis method eliminates potential dangerous accident caused by local overheating.And the raw materials were fed in solution by the peristaltic pump in distant place which improved the process safety.