Synthesis
3,4-Dimethyldiphenylamine can be synthesised electrochemically. The synthesis procedure is as follows:
To a 25 mL electrolytic cell, add 0.2 mmol of 3,4-dimethyldiphenylhydrazine, 0.2 mmol of hydrochloric acid, 0.4 mmol of lithium acetate, and 6 mL of N,N-dimethylacetamide. Under ambient conditions at room temperature, with continuous stirring using a magnetic stir bar, insert tin foil as both the anode and cathode into the cell and allow the reaction to proceed for 6 hours at a constant current of 12 mA, monitoring progress via TLC; Upon completion of the reaction, the reaction mixture was quenched with water, extracted with ethyl acetate, back-extracted with saturated saline solution, dried over anhydrous sodium sulphate, and subjected to reduced-pressure distillation at 45 °C. The residue was purified by rapid silica gel column chromatography (ethyl acetate: petroleum ether = 10:1) to obtain the product 3,4-dimethyldiphenylamine, with a yield of 93%.
