Preparation method of acetyl glycyrrhetinic acid
A technology of glycyrrhetinic acid and monoammonium glycyrrhizinate, which is applied in the fields of steroids and organic chemistry, can solve the problems of large organic solvent loss, cumbersome preparation process, and high cost. low cost effect
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[0033] Example 1
[0034] A preparation method of acetylglycyrrhetinic acid is prepared by the following steps:
[0035] Take 100kg of dried glycyrrhizic acid monoammonium salt mother liquor, add 450kg of glacial acetic acid with a concentration of 85%, stir and dissolve to obtain a mixed solution, then add 20kg of sulfuric acid to the mixed solution, heat up to 90 ° C, and react for 1.5h to carry out hydrolysis and acetylation reaction, After the above-mentioned reaction was completed, the temperature of the reaction system was reduced to 40 ℃ by feeding cooling water, filtered, washed successively with the glacial acetic acid of 65% with 100kg concentration, washed to pH 5 with water again, and dried at 85 ℃ to obtain acetylglycyrrhetinic acid 10.8 kg.
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[0036] Example 2
[0037] A preparation method of acetylglycyrrhetinic acid is prepared by the following steps:
[0038] Take 120kg of dry glycyrrhizic acid monoammonium salt mother liquor, add 550kg of glacial acetic acid with a concentration of 85%, stir and dissolve to obtain a mixed solution, then add 30kg of sulfuric acid to the mixed solution, heat up to 95°C, and react for 1.5h to carry out hydrolysis and acetylation. After the above-mentioned reaction was completed, the temperature of the reaction system was reduced to 40 ℃ by feeding cooling water, filtered, washed successively with the glacial acetic acid of 65% with 120kg concentration, washed to pH 5.5 with water again, and dried at 85 ℃ to obtain acetylglycyrrhetinic acid 12.24 kg.
Example Embodiment
[0039] Example 3
[0040] A preparation method of acetylglycyrrhetinic acid is prepared by the following steps:
[0041] Take 220kg of the dry product of glycyrrhizic acid monoammonium salt mother liquor, add 1000kg of glacial acetic acid with a concentration of 85%, stir and dissolve to obtain a mixed solution, then add 60kg of sulfuric acid to the mixed solution, heat up to 98 ℃, and react for 1.5h to carry out hydrolysis and acetylation reaction, After the above-mentioned reaction is completed, the temperature of the reaction system is reduced to 40 ℃ by passing into cooling water, filtered, washed successively with 250kg concentration of glacial acetic acid that is 65%, washed to pH 6 with water again, and dried at 85 ℃ to obtain acetylglycyrrhetinic acid 22.5 kg.
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