A kind of organically synthesized carboxymethyllysine separation and purification method
A carboxymethyl lysine, separation and purification technology, which is applied in the field of silica gel column chromatography separation and purification for synthesizing carboxymethyl lysine, can solve the problems of low efficiency and cumbersome ion exchange chromatography separation and purification methods, and achieves improved purification. Efficiency, the effect of reducing the experimental cost
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[0060] Reductive amination reaction: Weigh 1.88g (10mmol) of N-acetyl-L-lysine and 1.47g (20mmol) of glyoxylic acid monohydrate into a 250mL round bottom flask and add 80mL of 0.1mol / L Na 2 CO 3 Solution dissolved, continue to add 6.5g reducing agent NaBH 3 CN was placed in the reaction system, after the air in the reaction device was evacuated, nitrogen protection was introduced, and the reaction was carried out at 37°C for 20h. .
[0061] Esterification reaction: After the reaction is over, slowly add enough 37% concentrated hydrochloric acid to the reaction solution to remove excess unreacted NaBH 3CN, concentrated under reduced pressure in vacuo, and recovered the solvent to dryness. Add 40 mL of 3 mol / L hydrochloric acid n-butanol solution to dissolve the dried residue, mix well, and vacuum filter through a 0.45 μm organic filter to remove undissolved salt. The obtained clear solution was reacted at 65°C for 2h under constant stirring. After the reaction was complete...
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