Synthesis
Dissolve 52.3 g (0.44 mol) of sulfoxide chloride in 10 mL of chloroform in a four-necked flask equipped with a reflux condenser tube and an ice-water bath, stir mechanically, and use water to absorb the tail gas. The mixture of diethanolamine 21.5g (0.2 mol) and 15mL chloroform was slowly added dropwise, and the temperature of the reaction solution was controlled not to exceed 30 during the dropwise process, and the dropwise time was 3 h. After the dropwise process was completed, the ice-water bath was withdrawn, and the reaction was carried out at room temperature for 1 h. Then the temperature was slowly increased, and the temperature was raised to 50 when the solid was completely dissolved and the reaction was continued for 0.5 h. After the reaction was stopped and the reaction was cooled down to room temperature, and then the solid was filtered, and a white and yellowish green solid was obtained. Yellowish green solid, recrystallized with anhydrous ethanol, obtained white needle-like crystals. Dissolve ,-dichlorodiethylamine hydrochloride (12.7 g, 0.07 mol) in 55 mL of water, placed in a four-necked flask equipped with a reflux condenser tube, mechanical stirring, heating so that the solid was completely dissolved, dropwise addition of 0.07 mol of substitution of aniline, the pH was detected once every half an hour, dropwise addition of 50% aqueous sodium carbonate, so that the pH of the reaction system was maintained at 6, and the final pH no longer decreases. Stop heating, leave to cool to room temperature, filtration, the filter cake was washed twice with water and anhydrous ethanol, drying, to obtain white crystals.
