Method for removing solvent residues of diammonium glycyrrhizinate bulk drug
A technology of diammonium glycyrrhizinate and API, applied in steroids, organic chemistry and other directions, can solve problems such as deterioration, difficulty in reaching, darkening in color, etc., and achieve the effects of simple operation, high purity and improved product quality
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Embodiment 1
[0019] Put 60 g of crude diammonium glycyrrhizinate and 240 g of 50% ethanol solution into a 500 ml four-necked reaction flask, heat to 65°C to dissolve, add 2.2 g of activated carbon to decolorize for half an hour, and remove the activated carbon by hot filtration. After the filtrate is heated and dissolved, it is cooled to 50°C, added with treated seeds, stirred to cool down for crystallization, a small amount of crystals are precipitated at 47°C, continue to stir, stand at 40°C for crystallization, overnight, and the next day with ice water to cool down to 0~ 5°C, centrifugal filtration to obtain 84.6 g of wet product of diammonium glycyrrhizinate. The obtained wet product was dried under reduced pressure at 55° C. for 6 hours to obtain 49.2 g of primary dry product of diammonium glycyrrhizinate. The obtained primary dry product was placed under the condition of 70% air humidity for 10 hours, and the material weighed 53.2 g after moisture absorption. After the obtained mat...
Embodiment 2
[0021] Put 60 g of crude diammonium glycyrrhizinate and 240 g of 50% ethanol solution into a 500 ml four-necked reaction flask, heat to 65°C to dissolve, add 2.2 g of activated carbon to decolorize for half an hour, and remove the activated carbon by hot filtration. After the filtrate is heated and dissolved, it is cooled to 50°C, added with treated seeds, stirred to cool down for crystallization, a small amount of crystals are precipitated at 47°C, continue to stir, stand at 40°C for crystallization, overnight, and the next day with ice water to cool down to 0~ 5°C, centrifugal filtration to obtain 86.8 g of wet product of diammonium glycyrrhizinate. The obtained wet product was dried under reduced pressure at 55° C. for 7 hours to obtain 48.8 g of a primary dry product of diammonium glycyrrhizinate. The obtained primary dry product was placed under the condition of 80% air humidity for 16 hours, and the material weighed 53.7 g after moisture absorption. The obtained materia...
Embodiment 3
[0023] Put 60 g of crude diammonium glycyrrhizinate and 300 g of 55% ethanol solution into a 500 ml four-necked reaction flask, heat to 65°C to dissolve, add 2.2 g of activated carbon to decolorize for half an hour, and remove the activated carbon by hot filtration. After the filtrate is heated and dissolved, it is cooled to 52°C, added with treated seed crystals, stirred to cool down for crystallization, a small amount of crystals are precipitated at 47°C, continue to stir, stand at 40°C for crystallization, overnight, and the next day with ice water to cool down to 0~ 5°C, centrifugal filtration to obtain 90.1 g of wet product of diammonium glycyrrhizinate. The obtained wet product was dried under reduced pressure at 55° C. for 8 hours to obtain 48.0 g of a primary dry product of diammonium glycyrrhizinate. The obtained primary dry product was placed under the condition of 80% air humidity for 24 hours, and the material weighed 53.5g after moisture absorption. After the obt...
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