Preparation method of N,N-dimethyl-3-hydroxy-3-aryl propyl amine
A technology of aryl propylamine and aryl allyl amine, which is applied in the field of N, can solve the problems of low Mannich reaction yield, complex operation, and long reaction time, and achieve the effects of easy industrial production, simple preparation process, and short reaction time
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Embodiment 1
[0016] Add 2-acetthiophene (50.5g, 0.4mol), DMFDMA (95.2g, 0.8mol) and N,N-dimethylformamide (250ml) into the reaction flask, raise the temperature to 100°C and react for 3 hours, and then evaporate under reduced pressure. The solvent was cooled to obtain yellow crystals, which were recrystallized with ethyl acetate (400ml) to obtain light yellow crystals of N,N-dimethyl-3-oxo-3-(2-thienyl)propenamine (67.4g, 92.1) %). mp.117~119℃. MS m / z: 180.9, 148.0, 110.9, 98.0, 55.0, 42.0.
Embodiment 2
[0018] Lithium aluminum hydride (38g, 1.0mol) and tetrahydrofuran (300ml) were added to the reaction flask, and N,N-dimethyl-3-oxo-3-(2-thienyl)propenamine (36.2g, 0.2mol), after the addition, react at room temperature for 10 hours. Under cooling, slowly add water (200ml), continue to stir for 30 minutes, filter, extract the filtrate with dichloromethane (100ml×3), dry, filter, and evaporate the solvent to obtain a shallow Yellow viscous oil N,N-dimethyl-3-hydroxy-3-(2-thienyl)propylamine (33.5g, 82.4%), cooled and solidified to obtain a white solid, mp. 70-73°C. MS m / z: 185.1, 113.0, 85.0, 58.1, 30.1.
Embodiment 3
[0020] Add acetophenone (60.0, 0.5), DMFDMA (119g, 1.0mol) and N,N-dimethylformamide (300ml) into the reaction flask, heat up to 100°C and react for 4 hours, distill off the solvent under reduced pressure and cool to obtain yellow Crystallized and recrystallized from ethyl acetate (450ml) to give light yellow crystals of N,N-dimethyl-3-oxo-3-phenylpropenamine (78.9g, 90.1%). mp.93~94℃. MS m / z: 175.0, 158.0, 131.0, 98.0, 77.0, 42.0.
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