Preparation method of Beta-amino acid
A technology for amino acids and preparation steps, which is applied in the field of preparation of β-amino acids, can solve problems such as inconvenient operation, many synthesis steps, and instability, and achieve the effects of easy industrial production, simple process, and easy purification
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Embodiment 1
[0033] Add 28.1g (0.2mol) of 4-chlorobenzaldehyde and 120mL of ethanol into a 500mL autoclave, tighten the autoclave, and check the airtightness. Replace the air in the autoclave with nitrogen, feed ammonia, and start heating and stirring when the pressure reaches 0.66MPa. Control the reaction temperature at 95°C and react for 15 hours. The pressure will gradually increase at the beginning of the reaction, and the pressure will decrease at the end of the reaction. When the pressure of the autoclave is constant, cool down to room temperature, release the pressure, open the autoclave, add the reaction solution obtained above and 23g (0.22mol) of malonic acid into a 250mL three-necked flask, and continue under mechanical stirring. The reaction was heated at 95 °C for 10 h. Stop the reaction, cool the reaction mixture to room temperature, filter with suction, wash the solid thoroughly with 50 mL of distilled water, and dry to obtain a white powder product with a yield of 79.4%. ...
Embodiment 2
[0035] Add 42.2g (0.3mol) of 4-chlorobenzaldehyde and 150mL of ethanol into a 500mL autoclave, tighten the autoclave, and check the airtightness. Replace the air in the autoclave with nitrogen, feed ammonia, and start heating and stirring when the pressure reaches 0.70 MPa. Control the reaction temperature at 95°C and react for 15 hours. The pressure will gradually increase at the beginning of the reaction, and the pressure will decrease at the end of the reaction. When the pressure of the autoclave was constant, the temperature was cooled to room temperature, the pressure was released, the autoclave was opened, the reaction solution obtained above and 34.3g (0.33mol) malonic acid were added together in a 250mL three-necked flask, mechanically stirred, The reaction was heated at 70 °C for 10 h. Stop the reaction, cool the reaction mixture to room temperature, filter with suction, wash the solid thoroughly with 80 mL of distilled water, and dry to obtain a white powder produc...
Embodiment 3
[0037] Add 21.2g (0.2mol) of benzaldehyde and 120mL of ethanol into a 500mL autoclave, tighten the autoclave, and check the airtightness. The air in the autoclave was replaced with nitrogen, and ammonia gas was introduced. When the pressure rose to 0.72MPa, the temperature was raised and stirred. The reaction temperature was controlled at 85°C, and the reaction was carried out for 12 hours. The pressure will gradually increase at the beginning of the reaction, and the pressure will decrease at the end of the reaction. When the pressure of the autoclave is constant, cool down to room temperature, release the pressure, open the autoclave, add the reaction solution obtained above and 23g (0.22mol) of malonic acid into a 250mL three-necked flask, and continue under mechanical stirring. The reaction was heated at 85 °C for 10 h. Stop the reaction, cool the reaction mixture to room temperature, filter with suction, wash the solid thoroughly with 50 mL of distilled water, and dry ...
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