The invention provides a preparation method of a herbicide oxadiazon intermediate 2, 4-dichloro-5-isopropoxy phenylhydrazine, which comprises the following steps: by taking a toluene solution of 2, 4-dichloro-5-isopropoxy aniline as a raw material, stirring to form a salt under an acidic condition, reacting with cyanate at a certain temperature to generate urea, degrading and rearranging by Hofmann in an alkaline environment, filtering, after recovering a solvent at normal pressure, taking 2, 4-dichloro-5-isopropoxy phenylhydrazine as a raw material, adding chloroform for extraction, and obtaining a chloroform solution of the 2, 4-dichloro-5-isopropoxy phenylhydrazine which can be directly used for an acylation process to synthesize the oxadiazon key intermediate 2, 4-dichloro-5-isopropoxy phenylhydrazine. According to the method disclosed by the invention, a complicated tin recovery process caused by reduction of diazonium salt by stannous chloride in a traditional synthesis process is effectively avoided, and generation of a large amount of high-salt wastewater in a recovery section is avoided; on the other hand, alkalization operation is avoided, solid materials are not added, the labor intensity is greatly reduced, and the production efficiency is effectively improved.