This invention relates to a method for preparing 2-nitro-5-cyanothiobenzoic acid, comprising: (1) dissolving 5-amino-2-
nitrobenzoic acid and an acid in a first reaction
solvent, water, adding a nitrosating agent dropwise to the
reaction system, reacting at a temperature of -20 to 20°C for 1 to 12 h, to obtain intermediate 3-carboxy-4-
nitrobenzene diazonate M; the first reaction
solvent is one or a mixture of water,
acetonitrile, and
ethanol; (2) reacting the intermediate 3-carboxy-4-
nitrobenzene diazonate M obtained in step (1) with a thiocyanating agent and a catalyst in a second reaction
solvent to undergo a
nucleophilic substitution reaction, reacting at a temperature of -20 to 30°C for 1 to 24 h, to obtain 2-nitro-5-cyanothiobenzoic acid; the thiocyanating agent is selected from one or a mixture of
cuprous thiocyanate,
sodium thiocyanate, or
potassium thiocyanate; the second reaction solvent is one or a mixture of water,
acetonitrile, and
ethanol. The raw materials of this invention are readily available, the cost is controllable, the reaction is mild, it is green and
environmentally friendly, and it has
high selectivity and high yield.