This invention discloses a method for synthesizing 4-fluoro-3,5-dimethylphenylhydrazine
hydrochloride, belonging to the field of pharmaceutical intermediate synthesis technology. The synthesis method involves the following steps:
copper halide, hydrazine additives acting as catalysts, a
phase transfer catalyst, K3PO4, and 4-fluoro-3,5-dimethylbromobenzene are added to a
solvent, and the temperature is raised to 80℃-100℃; hydrazine
hydrate is added dropwise to the above mixture, and after the addition is complete, the temperature is maintained at 80℃-100℃ for 6-10 hours; after the reaction is complete, the temperature is lowered to
room temperature,
dichloromethane is added, the mixture is filtered, and the filtrate is separated, the aqueous layer is removed, and the
organic layer is washed with saturated brine; the washed organic phase is acidified to pH 2-3 to obtain crude 4-fluoro-3,5-dimethylphenylhydrazine
hydrochloride; the crude product is recrystallized to remove impurities, yielding a finished product with a purity of over 99%. This invention utilizes readily available raw materials, achieves high yield, produces a high-purity finished product, has a simple preparation method, a short
processing cycle, and low manufacturing cost.