The application relates to the
fine chemical technology field and discloses a method for synthesizing N,O-dimethyl-N'-nitroisourea, which specifically comprises the following steps: mixing
urea and an
imidazole ionic liquid, adding
dimethyl carbonate drop by drop under temperature rising, performing heat preservation reaction, opening a vacuum, continuously removing low-boiling substances in a slow temperature rising process, cooling, stirring, adding fuming
nitric acid drop by drop, stirring and temperature rising, performing heat preservation reaction, cooling and standing to separate
layers, pumping the upper concentrated
nitric acid into
nitrogen dioxide and
oxygen, waiting for reuse, adding 4-6 times of water into the lower
ionic liquid and N,O-dimethyl-N'-nitroisourea mixture, stirring and temperature rising, separating
layers, taking the upper layer of N,O-dimethyl-N'-nitroisourea-containing
aqueous solution, slowly cooling, precipitating white solids, filtering, washing with
ice water,
drying, and obtaining N,O-dimethyl-N'-nitroisourea, so that the shortcomings of traditional
synthesis methods, i.e. the necessity of using
dimethyl sulfate and
sulfuric acid to generate dangerous waste salt of
sodium sulfate and waste mixed acid with high COD, are solved.