1,3-Propanediamine, N1,N3-di-2-propen-1-yl-, hydrochloride (1:2)

Preparation

The preparation of 1,3-Propanediamine, N1,N3-di-2-propen-1-yl-, hydrochloride (1:2) is as follows:The 2L reaction kettle was heated to 5 degrees Celsius under nitrogen protection, 800.6 g of 3-aminopropene was added to the reaction kettle, and 200.1 g of 1,3-dichloropropane was added to the dropping tank.The reaction kettle was heated to 50 degrees Celsius, 1,3-dichloropropane was added dropwise to the reaction kettle, and after the addition was completed, the temperature of the reaction system was controlled to react at 85 degrees Celsius.During the dropwise addition and reaction, the reaction pressure is not higher than 0.35MPa, and the GC purity of the raw material 1,3-dichloropropane is 0.The temperature was lowered to below 40 degrees Celsius, and the reaction pressure was distilled into the concentration kettle by nitrogen pressing, and 502.1 g of 3-aminopropene fraction was separated by atmospheric pressure distillation at 30 to 80 degrees Celsius. The residual 3-aminopropene was distilled under elevated temperature and reduced pressure.After the underpressure distillation finishes, lower the temperature, transfer the distillation residue to the crystallization kettle, and within 5 degrees Celsius, slowly dropwise add the hydrochloric acid-isopropanol solution configured in advance in the crystallization kettle (hydrochloric acid: isopropyl alcohol=200.0g: 600.0 g), adjust the pH of the system to 1.6, and keep for 2 hours for crystallization.After crystallization, the crude product of N,N'-diallyl 1,3-propanediamine dihydrochloride was obtained by filtration and separation.b. PurificationThe crude N,N'-diallyl 1,3-propanediamine dihydrochloride obtained above was added with 600.0 g of isopropanol to disperse, stirred and beaten at room temperature for 2 hours, and after the crystallization was completed, filtered and separated to obtain N ,N'-diallyl 1,3-propanediamine dihydrochloride wet product, put the wet product into a vacuum desiccator to dry, after drying, a high-purity qualified product 308.8g, GC purity 99.8%, was obtained. rate 73.1%.