The invention discloses a method for preparing 6-nitrobenzofuroxan by a one-pot method, which comprises the following steps: firstly, mixing 2, 4-dichloro-1, 3, 6-trinitrobenzene and monobasic
organic acid according to a
mass ratio of 1: (8-20) until the 2, 4-dichloro-1, 3, 6-trinitrobenzene and the monobasic
organic acid are dissolved; the preparation method comprises the following steps: mixing 2, 4-diazido-1, 3, 6-trinitrobenzene and 2, 4-dichloro-1, 3, 6-trinitrobenzene according to a
molar ratio of 1: (0.5-2), adding
sodium azide into a
mixed solution obtained in the step 1, and reacting at 20-50 DEG C for 0.5-2 hours to obtain an acid solution of 2, 4-diazido-1, 3, 6-trinitrobenzene, with the
molar ratio of 2, 4-dichloro-1, 3, 6-trinitrobenzene to
sodium azide being 1: (0.5-2); then, the temperature of the acid solution of the 2, 4-diazido-1, 3, 6-trinitrobenzene is increased to 70 DEG C to 120 DEG C, and a reaction is conducted for 0.5 h to 3 h at the temperature; and finally, carrying out rotary
evaporation on the reaction liquid, removing the monobasic
organic acid to obtain orange
powder, adding water, washing, filtering and
drying to obtain the 6-nitrobenzofuroxan. According to the preparation method disclosed by the invention, the 6-nitrobenzofuroxan can be obtained by carrying out azidation reaction and
pyrolysis condensation reaction on 2, 4-dichloro-1, 3, 6-trinitrobenzene only by using one
organic solvent, so that the generation of organic waste liquid is greatly reduced.