What problems should be paid attention to when synthesizing N,N-Dihydroxyethylglycine (Bicine)?
Release time:
2021-06-17
The compound N,N-Dihydroxyethylglycine (Bicine) is a pH buffer suitable for biochemical and medical research. This property makes Bicine often used as a buffer solution for capillary electrophoresis. Desheng is a manufacturer of Bicine, so it has certain experience in the production process. The matters needing attention in the production and synthesis process are organized as follows:
The influence of nitrogen
Add 35.05 g of diethanolamine (0.3 mol) and 48.33 g of 40% glyoxal aqueous solution (0.3 mol) into a 250 ml three-necked flask, raise the temperature to 95 ℃, and react for 2 h. Under the same conditions, the yield (82.48%) of the product obtained by the reaction conditions with nitrogen gas is higher than the yield (76.24%) obtained by the reaction conditions without nitrogen gas. This is because diethanolamine is easily oxidized in air. Under the protection of nitrogen, it can effectively prevent diethanolamine from being oxidized by air, so that it can better react with glyoxal, so the reaction yield is higher.
The influence of reactant molar ratio
Under nitrogen conditions, a certain amount of diethanolamine was added to a 40% glyoxal aqueous solution, and then the temperature was raised to 95 ℃ for 2 h. Under the same conditions, when the molar ratio is 1:1, the yield of the reaction is the highest.
The effect of reaction time
Under nitrogen conditions, 0.3 mol of diethanolamine was mixed with an equimolar amount of 40% glyoxal aqueous solution, and the temperature was raised to 95 ℃ for a certain period of time. Under the same conditions, with the prolongation of the reaction time, the yield of Bicine gradually increases, but it will level off after a certain period of time. So when the reaction time is 90 minutes, the yield of Bicine reaches its maximum.
Effect of reaction temperature
Under nitrogen conditions, 0.3 mol of diethanolamine was mixed with an equimolar amount of 40% glyoxal aqueous solution, then the temperature was raised, and the reaction was continued for 2 h at a certain temperature. Under the same conditions, as the reaction temperature increases, the yield of Bicine gradually increases, because as the temperature increases, the reaction activity of the reactants increases. But when the reaction temperature increases to a certain extent. The yield will no longer change. When the reaction temperature is 95 ℃, the reaction yield is the highest. The appearance of the obtained product is white needle-like crystals, and the melting point is 192～194 ℃.
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