Take 4-ethoxyaniline (2.19mol) and 309.2g triethylamine (3.06mol) in a 5000mL three-mouth round bottom flask, add 1000mL of ethyl acetate, cooled in an ice bath and stirred mechanically. When the temperature of the mixture was reduced to 0 ~5 , 299.2 g of CS2 (3.93 mol) was added slowly by dropping with a constant pressure dropping funnel, and the temperature of the reaction solution was controlled to be below 30 by magnetic stirring while dropping. After the dropwise addition, the reaction solution was stirred magnetically at room temperature (10-30 range) for one hour; at this temperature, 299.2 g of CS2 (3.93 mol) and DMAP catalyst were added to the reaction solution, and the reaction was stirred at 30±2.5 for 1.5 h. At the end of the reaction, the reaction solution was washed with an acid solution twice, and the total amount of acid consumed for washing was 1.5 times that of triethylamine, and washed to neutrality with saturated saline. The reaction solution was washed with acid solution twice, the total acid consumption was 1.5 times of triethylamine, and then washed with saturated saline to neutral. The organic phase was evaporated and concentrated to obtain 2-ethoxyphenyl isothiocyanate.