The general procedure for synthesizing 2-(dimethylamino)acetal sulfite from dimethylaminoacetaldehyde diethyl acetal was as follows: 40.0 g of dimethylaminoacetaldehyde diethyl acetal was added to a mixture comprising 48.0 g of concentrated hydrochloric acid and 20.0 mL of water, heated to 40°C and maintained at this temperature for 3 hours of reaction. Subsequently, a solution of 42.4 g of sodium bisulfite dissolved in 72.0 mL of water (aqueous sodium bisulfite) was slowly added dropwise, and stirring of the reaction mixture was continued for 1 hour after completion of the dropwise addition. 200.0 mL of ethanol was added to the reaction system and the mixture was subsequently stirred at 0°C for 2 hours. Upon completion of the reaction, the suspension was separated by filtration, and the solid product was washed with 160.0 mL of ethanol and dried under vacuum at 45 °C. A final product of 42.5 g was obtained in 89.6% yield of the theoretical value. The product started to decompose at 180°C.
