preparation | dissolve 52.3g(0.44mol) thionyl chloride in 10mL chloroform, place it in a four-mouth flask equipped with reflux condenser tube and ice water bath, stir mechanically, and absorb tail gas with water. Slowly drop the mixed solution of 21.5g(0.2mol) of diethanolamine and 15mL of chloroform. During the drop process, the temperature of the reaction solution is controlled not to exceed 30 ℃, and the drop time is 3h. After dropping, remove the ice water bath, react at room temperature for 1h, then slowly raise the temperature, after the solid is completely dissolved, raise the temperature to 50 ℃, continue the reaction for 0.5h, stop heating, cool to room temperature, filter, get white yellowish green solid, recrystallized with absolute ethanol, get white needle-like crystals. Dissolve β, β'-dichlorodiethylamine hydrochloride (12.7g,0.07mol) in 55mL of water, place it in a four-port flask equipped with reflux condenser tube, mechanically stir, heat to completely dissolve the solid, dropwise 0.07mol of substituted aniline, detect pH once every half hour, dropwise 50% sodium carbonate aqueous solution, keep the pH of the reaction system at 6, finally the pH no longer decreases, and stop heating, let it stand and cool to room temperature, filter, wash the cake twice with water and anhydrous ethanol, and dry to obtain white crystals. |