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• Synthesis

  

  Place 100g of 4-chloro-2-nitrotoluene and 20g of vanadium pentoxide together in a 1000mL three-necked flask. Add 740g of pre-prepared 75% sulfuric acid solution to the three-necked flask. Install a thermometer, reflux separator, dropping funnel, condenser, stirrer, exhaust gas absorption device, and vacuum device. Heat the reaction solution to the required temperature under stirring. Turn on the vacuum device to maintain a slight negative pressure in the reaction system to facilitate the discharge of exhaust gas. Maintain the reaction temperature and pressure under stirring, and slowly add 110mL of 65% concentrated nitric acid in 11h to the reaction mixture.

  During the dropwise addition of nitric acid, some of the raw materials distill off as an azeotrope with water. The resulting distillate separates into layers upon condensation; the oil phase is returned to the reactor, and the aqueous phase is discharged. After the reaction is complete, the reaction conditions are maintained, and stirring continues for 1 L. The reaction solution is cooled to 100–120 °C, and 250 mL of extractant is added. The system temperature is maintained, and the mixture is stirred for 30 min and allowed to stand. The mixture separates into layers, and the aqueous phase is returned to the flask as the mother liquor for the next reaction. The oil phase is cooled to room temperature and filtered. The filter cake is vacuum dried at 50 °C to obtain crude 4-chloro-2-nitrobenzoic acid. The crude 4-chloro-2-nitrobenzoic acid is recrystallized from chlorobenzene and vacuum dried at 50 °C to obtain a product with a purity greater than 99%, which is a white crystalline powder.;

• Application

  4-Chloro-2-nitrobenzoic acid, also known as p-chloro-o-nitrobenzoic acid, is an important organic intermediate used in the production of pesticides, pharmaceuticals, dyes, and many other products. 4-Chloro-2-nitrobenzoic acid can be obtained by the oxidation of 4-chloro-2-nitrotoluene.;

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