Improved method for synthesis process of manidipine hydrochloride
A manidipine hydrochloride and synthetic process technology, applied in the direction of organic chemistry, can solve the problems of low product purity, complexity and unsuitability for industrial production, and achieve the effects of reducing costs, shortening production cycle, and simple operation
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Embodiment 1
[0019] Step 1: Add 1.22kg (4.12mol) 1-benzhydryl-4-(2-hydroxyethyl)piperazine (IV) into the reaction flask, heat to 70-75°C, add dropwise 0.43kg ( 5.12mol) of diketene, after dropping, keep stirring at 70-80°C for 2h. After the reaction was completed, 6L of ethyl acetate was added for dissolution, and the organic phase was washed with water for 3 times, dried, and concentrated to obtain oily substance 2-(4-benzhydryl-1-piperazinyl) ethyl acetoacetate (III) 1.50 kg (yield: 95.8%).
[0020] Step 2: 1.50kg (3.94mol) of the above-mentioned oil (III) and 0.45kg (3.91mol) of methyl 3-aminocrotonate, 0.59kg (3.90mo) of m-nitrobenzaldehyde, and 4.95kg of isopropanol are dissolved in In a 10L reaction flask, heat and reflux for 7 hours, distill out isopropanol, add 15L ethyl acetate to the residue to dissolve, wash with water, separate liquid, concentrate, add 3L methanol to dissolve, adjust the pH value of the system to between 1-2 with concentrated hydrochloric acid 15L ethyl aceta...
Embodiment 2
[0023] Step 1: Add 1.22kg (4.12mol) 1-benzhydryl-4-(2-hydroxyethyl)piperazine (IV) into the reaction flask, heat to 70-75°C, add dropwise 0.43kg ( 5.12mol) of diketene, after dropping, keep stirring at 70-80°C for 2h. After the reaction was completed, 8 L of methyl acetate was added for dissolution, and the organic phase was washed with water three times, dried, and concentrated to obtain 1.47 kg of oil (III) (yield: 93.9%).
[0024] Step 2: Dissolve 1.1.47kg (3.86mol) of the above-mentioned oil (III) and 0.44kg (3.82mol) of methyl 3-aminocrotonate, 0.58kg (3.84mo) of m-nitrobenzaldehyde, and 4.95kg of isopropanol In a 10L reaction flask, heat and reflux for 7 hours, distill out isopropanol, add 17L methyl acetate to the residue to dissolve, wash with water, separate liquid, concentrate, add 3L methanol to dissolve, adjust the pH value of the system to 1-2 with concentrated hydrochloric acid 17L methyl acetate to dissolve the filter cake, adjust the pH value of the system wit...
Embodiment 3
[0027] Step 1: Add 1.22kg (4.12mol) 1-benzhydryl-4-(2-hydroxyethyl)piperazine (IV) into the reaction flask, heat to 70-75°C, add dropwise 0.43kg ( 5.12mol) of diketene, after dropping, keep stirring at 70-80°C for 2h. After the reaction was completed, 6L of ethyl acetate was added for dissolution, and the organic phase was washed with water for 3 times, dried, and concentrated to obtain oily substance 2-(4-benzhydryl-1-piperazinyl) ethyl acetoacetate (III) 1.52 kg (yield: 97.1%).
[0028] Step 2: 1.50kg (3.94mol) of the above-mentioned oil (III) and 0.45kg (3.91mol) of methyl 3-aminocrotonate, 0.59kg (3.90mo) of m-nitrobenzaldehyde, and 4.95kg of isopropanol are dissolved in In a 10L reaction flask, heat and reflux for 7 hours, distill out isopropanol, add 15L ethyl acetate to the residue to dissolve, wash with water, separate liquid, concentrate, add 3L methanol to dissolve, adjust the pH value of the system to between 1-2 with concentrated hydrochloric acid 15L ethyl aceta...
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