Preparation process of organic acid lithium-L-proline salt
A technology of proline salt and organic acid lithium, applied in the field of preparation technology of organic acid lithium-L-proline salt, can solve the problems of metabolic acidosis, aggravating kidney burden, blood pH value disorder, etc. Degenerative disease, prevention of suicide risk, efficacy of enhanced efficacy
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Embodiment 1
[0024] Embodiment 1, the preparation technology of a kind of organic acid lithium-L-proline salt described in the present invention, tests the dissolubility of lithium isobutyrate, L-proline in the following solvents, judges lithium isobutyrate, Good and poor solvents for L-proline.
[0025] Take 1 mg of solute, add 100 μL of solvent, observe the dissolution, if insoluble, ultrasonically observe the dissolution for 2 minutes; if it is still insoluble, add 100 μL of solvent, observe the dissolution, if insoluble, ultrasonicate for 2 minutes and then observe the dissolution; Add solvent until the product is completely dissolved, record the total amount of solvent added, or stop the solubility test if the product is not dissolved after adding up to 1 mL, so as to judge the good solvent and poor solvent of lithium isobutyrate and L-proline .
[0026] As shown in the table below, the solubility test results of lithium isobutyrate and L-proline
[0027]
Embodiment 2
[0028] Embodiment 2, the preparation process of a kind of organic acid lithium-L-proline salt according to the present invention, adopts single solvent crystallization method to prepare lithium isobutyrate-L-proline salt, the operation steps are as follows:
[0029] Add an appropriate amount of good solvent n-butanol to the equivalent chemical equivalent of lithium isobutyrate and L-proline, dissolve it just under heating and reflux and record the amount of solvent used, stir for about 3 hours, filter while it is hot, and naturally cool and analyze Crystal, filter the solid, vacuum dry to constant weight to obtain 589.3mg white solid, the mass yield is 53.06%, send XRD and hydrogen spectrum inspection
[0030] Proton spectrum data: Deuterated reagent is: CD 3 OD
[0031] combined with Figure 1~4 , draw: the chemical equivalent ratio of lithium isobutyrate and L-proline in the precipitated solid under n-butanol is 1:1; in view of the solubility of lithium isobutyrate and L-p...
Embodiment 3
[0037] Example 3, a preparation process of organic acid lithium-L-proline salt according to the present invention, using a mixed solvent crystallization method to prepare lithium isobutyrate-L-proline salt
[0038] Add an appropriate amount of good solvent to the equivalent chemical equivalent of lithium isobutyrate and L-proline, heat and reflux to make it just dissolve, then add an appropriate amount of poor solvent until the solid is just precipitated, add a good solvent to re-dissolve, and reflux for 3 h, natural cooling and crystallization, filtering the solid, vacuum drying to constant weight to obtain 374.8mg white solid, the mass yield is 33.75%, send XRD and hydrogen spectrum inspection
[0039] Proton spectrum: deuterated reagent is: CD 3 OD
[0040] combined with Figure 9 And attached Figure 1~3 , the analysis shows that: the chemical equivalent ratio of lithium isobutyrate and L-proline in ethanol and tetrahydrofuran mixed solvent precipitation solid is 1:1; ...
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