Synthesis
The general procedure for the synthesis of sodium ethylsulfite from ethylsulfonyl chloride was as follows: sodium sulfite (53.9 g, 0.428 mol), sodium bicarbonate (65.34 g, 0.778 mol), and deionized water (325 mL) were added to a four-necked flask equipped with a stirrer at room temperature and under nitrogen protection. The reaction mixture was stirred continuously at 80 °C for 1.3 hours. Subsequently, ethanesulfonyl chloride (50.0 g, 0.389 mol) was slowly added dropwise to the reaction system and the reaction continued to be stirred at the same temperature for 4.2 hours. Upon completion of the reaction, the reaction mixture was concentrated by rotary evaporator. Anhydrous ethanol was added to the concentrated residue and concentrated again. Next, toluene was added to the residue and the concentration process was repeated to completely remove water. The resulting solid was dried under vacuum, then anhydrous ethanol (100 mL) was added and the mixture was heated to reflux. The mixture was hot filtered and the solids were washed with a small amount of ethanol. All the filtrate and washings were combined and finally concentrated by rotary evaporator to give a white solid sodium ethylsulfite (38.96 g, yield calculated based on ethylsulfonyl chloride).
References
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[2] Chemistry - A European Journal, 2016, vol. 22, # 50, p. 18085 - 18091
[3] Macromolecules, 2018, vol. 51, # 20, p. 8188 - 8196
[4] Chemistry - A European Journal, 2016, vol. 22, # 25, p. 8694 - 8699
[5] Journal of Medicinal Chemistry, 1989, vol. 32, # 11, p. 2436 - 2442
