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

Inactive Publication Date: 2010-05-12
南京璇荣贸易有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the prior art, the extraction and separation method of galantamine mainly adopts organic solvent method, etc., but the content of galantamine obtained by these extraction processes is low, the pollution in the production process is serious, and it is unfavorable for large-scale production operations

Method used

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  • Method for preparing galanthamine

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Experimental program
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Effect test

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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Abstract

The invention relates to a method for preparing galanthamine, which has the advantages of simple and convenient operation, light pollution and less equipment investment, and comprises the following process steps: adding coarse powder of bulb of Lycoris into a CO2 supercritical extractor, taking 5 percent HCL-chloroform (1:1) as an entrainer which accounts for 2 to 6 volume percent of the total extraction solvent, controlling the extraction pressure to between 10 and 40MPa, the temperature to between 30 and 60DEG C, the CO2 flow rate to between 1 and 5ml / g crude medicament / min and the extraction time to between 150 and 250min, and obtaining an extractive matter; adding NaHCO3 to regulate pH to between 9 and 10, adding ethyl acetate in equal volume to extract for three times, combining ethyl acetate layers, adding anhydrous sodium sulfate for dehydration, filtering, and recovering solvent in the filter liquor at reduced pressure until the filter liquor is dry; and adding hot ethanol for dissolution, standing for crystallization, separating crystals, and adding absolute ethyl alcohol for recrystallization. By adopting the method for preparing the galanthamine, products have high purity, and industrial development is easy to implement.

Description

technical field [0001] The invention relates to a preparation method of galantamine, in particular to a method for extracting galantamine from plants. Background technique [0002] Galanthamine, synonym: galanthamine, molecular formula: C 17 h 21 NO 3 , molecular weight: 287.358, CAS accession number: 60384-53-4, the structural formula is as follows: [0003] [0004] Galantamine is a natural compound with a strong anti-senile dementia effect, which is mainly distributed in various plants of Amaryllidaceae. [0005] Lycoris is the bulb of Lycoris radiata (L.Herit.) Herb. It has detoxification, vomiting, detumescence, insecticidal and other effects. It contains a lot of galantamine. [0006] In the prior art, the extraction and separation methods of galantamine mainly use organic solvent methods, etc., but the content of galantamine obtained by these extraction processes is low, the pollution in the production process is serious, and it is not conducive to large-scal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/107
CPCY02P20/54
Inventor 张发成毛志英范淦彬
Owner 南京璇荣贸易有限公司
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