Method for preparing galanthamine
A galantamine, supercritical technology, used in bulk chemical production, organic chemistry, etc., can solve the problems of serious pollution, unfavorable large production operations, and low galantamine content
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Embodiment 1
[0019] Get Lycoris bulb meal 10Kg, add to CO 2 In the supercritical extractor, 5% HCL-chloroform (1: 1) is used as entrainer, and the volume percentage of entrainer to total extraction solvent is 2%, extraction pressure 10MPa, temperature 30 ℃, CO 2 The flow rate is 1ml / g crude drug / min, the extraction time is 150min, and the extract is obtained. Add NaHCO3 to adjust the pH to 9-10, add an equal volume of ethyl acetate to extract 3 times, combine the ethyl acetate layers, add anhydrous sodium sulfate for dehydration, filter, and take The filtrate was decompressed to recover the solvent to dryness, added hot ethanol to dissolve, left to crystallize, separated and crystallized, added absolute ethanol to recrystallize, separated, washed and dried to obtain 0.5 g of galantamine, which was detected by HPLC with a purity of 99.0%.
Embodiment 2
[0021] Get Lycoris bulb meal 10Kg, add to CO 2 In the supercritical extractor, 5% HCL-chloroform (1: 1) is used as the entrainer, and the volume percentage of the entrainer in the total extraction solvent is 6%, the extraction pressure is 40MPa, the temperature is 60°C, and the CO 2 The flow rate is 5ml / g crude drug / min, the extraction time is 250min, and the extract is obtained. Add NaHCO3 to adjust the pH to 9-10, add an equal volume of ethyl acetate to extract 7 times, combine the ethyl acetate layers, add anhydrous sodium sulfate for dehydration, filter, and take The filtrate was decompressed to recover the solvent to dryness, added hot ethanol to dissolve, left to crystallize, separated and crystallized, added absolute ethanol to recrystallize, separated, washed and dried to obtain 1.2 g of galantamine, which was detected by HPLC with a purity of 98.6%.
Embodiment 3
[0023] Get Lycoris bulb meal 10Kg, add to CO 2 In the supercritical extractor, 5% HCL-chloroform (1: 1) is used as the entrainer, and the entrainer accounts for 4% by volume of the total extraction solvent, the extraction pressure is 30MPa, the temperature is 45°C, and the CO 2 The flow rate is 2ml / g crude drug / min, the extraction time is 200min, and the extract is obtained. Add NaHCO3 to adjust the pH to 9-10, add an equal volume of ethyl acetate to extract 5 times, combine the ethyl acetate layers, add anhydrous sodium sulfate for dehydration, filter, and take The filtrate was decompressed to recover the solvent to dryness, added hot ethanol to dissolve, left to crystallize, separated and crystallized, added absolute ethanol to recrystallize, separated, washed and dried to obtain 1.3 g of galantamine, which was detected by HPLC with a purity of 99.6%.
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