Method for synthesizing methylaminopyridine compound by one-step method
A methylaminopyridine and compound technology, applied in the field of methylaminopyridine raw material synthesis, can solve problems such as being unsuitable for industrial production, high reaction conditions, and many three wastes pollution, and achieve convenient product separation and purification, lower production costs, and high yields Effect
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Embodiment 1
[0024] A method for synthesizing an aminopyridine compound in one step, comprising the following steps:
[0025] Use cyanopyridine as raw material, methanol as reaction solvent, and palladium carbon catalyst as catalyst. After nitrogen replacement, react for 4-10 hours under ammonia atmosphere, hydrogen pressure 0.5-2.0MPa, temperature 15-30°C, and cool to room temperature Filtrate, recover the filter residue for later use, and distill the filtrate under reduced pressure at 65°C and -0.1MPa to obtain the product aminopyridine compound;
[0026] Wherein, the mass ratio of cyanopyridine, methanol, palladium carbon catalyst, and ammonia is 1: (5-10): (0.01-0.05): (0.1-0.3);
[0027] The loading amount of palladium in the palladium-carbon catalyst is 5-10%, and the palladium-carbon catalyst prepared by the prior art can be used.
Embodiment 2
[0029] The method for synthesizing 4-methylaminopyridine by one-step method comprises the following steps:
[0030] (1) Add 200kg of 4-cyanopyridine and 1000kg of methanol into the pressure reactor, stir and dissolve and add 2kg of palladium-carbon catalyst with a palladium loading of 5%;
[0031] (2) After three replacements with nitrogen, 20kg of ammonia gas was introduced under stirring;
[0032] (3) Introduce hydrogen and react for 10 hours at a hydrogen pressure of 1.0MPa and a temperature of 30°C;
[0033] (4) After cooling to room temperature and filtering, the filter residue is recovered as a palladium carbon catalyst for later use; the filtrate is subjected to vacuum distillation at 65°C and -0.1MPa to obtain the product 4-methylaminopyridine, which is a colorless transparent viscous liquid, distilled out The reaction solvent methanol reclaims for subsequent use;
[0034] The yield of the product 4-methylaminopyridine was 82.65%, and its purity was 99.94% as detecte...
Embodiment 3
[0036] The method for synthesizing 4-methylaminopyridine by one-step method comprises the following steps:
[0037] (1) Add 200kg of 4-cyanopyridine and 1000kg of methanol into the pressure reactor, stir and dissolve and add 10kg of palladium-carbon catalyst with a palladium loading of 5%;
[0038] (2) After three replacements with nitrogen, 20kg of ammonia gas was introduced under stirring;
[0039] (3) Introduce hydrogen and react for 4 hours at a hydrogen pressure of 1.0MPa and a temperature of 30°C;
[0040] (4) After cooling to room temperature and filtering, the filter residue is recovered as a palladium carbon catalyst for later use; the filtrate is subjected to vacuum distillation at 65°C and -0.1MPa to obtain the product 4-methylaminopyridine, which is a colorless transparent viscous liquid, distilled out The reaction solvent methanol reclaims for subsequent use;
[0041] The yield of the product 4-methylaminopyridine was 89.93%, and its purity was 99.90% as detecte...
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