236750-65-5

80407-68-7

236750-65-5

The general procedure for the synthesis of 4,5-bis(2-methoxyethoxy)-2-nitrobenzonitrile from 3,4-bis(2-methoxyethoxy)benzonitrile was as follows: 1) Nitration reaction: 200g of 3,4-bis(2-methoxyethoxy)benzonitrile was dissolved in 3L of glacial acetic acid to prepare feedstock I. Concentrated sulfuric acid and concentrated nitric acid were used as feedstock II and feedstock III, respectively. the flow rate was adjusted by a flow pump so that the flow rate of feedstock I was 20 ml/min, that of feedstock II was 10 ml/min, and that of feedstock III was 6 ml/min. the flow rate was adjusted by a flow pump so that the flow rate of feedstock II was 10 ml/min, and the flow rate of feedstock III was 6 ml/min. It was ensured that the molar ratio of HNO3 to 3,4-bis(2-methoxyethoxy)benzonitrile was 1:1.5, and the mass ratio of concentrated nitric acid to concentrated sulfuric acid was 1:4. The reaction temperature was set at 60 °C, and the reaction residence time was set at 60 seconds. The temperature of the cooling module was set to 20 °C. The reaction solution from the outlet of the cooling module was collected and the glacial acetic acid was recovered by distillation under reduced pressure. The residue was added to 1.2 L of water and extracted twice with 1 L of ethyl acetate. The organic phases were combined, washed to neutrality with saturated sodium bicarbonate solution, dried over anhydrous sodium sulfate and evaporated. 215.21 g of 4,5-bis(2-methoxyethoxy)-2-nitrobenzonitrile was obtained with 90.58% yield and 98.95% purity.