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Fibrauretine preparation method

A technology of berberine and berberine, which is applied in the field of chemical drug preparation, can solve the problems of harsh reaction conditions, poor reaction selectivity, and unsuitability for industrial production, and achieve the effects of high product yield and purity, low cost, and simple process

Inactive Publication Date: 2013-11-27
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in actual operation, it is found that the reaction selectivity is poor, and the methylene group cannot be completely removed.
Another study used berberine to simultaneously demethylate and methylene through the aluminum chloride / toluene system, and then methylate dimethyl sulfate to obtain palmetine, but the process solvent toluene is highly toxic and the reaction Harsh conditions, not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take 3 g of berberine, add dichloromethane equivalent to 10 times the quality of berberine, and stir to obtain system A; add anhydrous aluminum chloride equivalent to 2.5 times the quality of berberine to system A, and stir until the solids Then viscous and evenly dispersed into small particles, then sealed and placed for 24 hours, then add hydrochloric acid equivalent to 10 times the quality of berberine and a concentration of 6mol / L, filter after stirring for 1 hour; filter again after the gained filtrate stands for 2 hours, and then Combine the precipitates obtained by filtering twice, then wash and dry the combined precipitates; take the precipitates after washing and drying, add acetone equivalent to 15 times the mass of the precipitates, and then add dropwise at room temperature Dimethyl sulfate of 1.5 times the mass of the precipitate, then add NaOH powder equivalent to 0.5 times the mass of the precipitate, and then heat and reflux for 5 hours under stirring; aft...

Embodiment 2

[0016] Get 7g of berberine, add dichloromethane equivalent to 10 times the quality of berberine, and stir to obtain system A; add anhydrous aluminum chloride equivalent to 2.5 times the quality of berberine to system A, and stir until the solids Then viscous and evenly dispersed into small particles, then sealed and placed for 24 hours, then add hydrochloric acid equivalent to 10 times the quality of berberine and a concentration of 6mol / L, filter after stirring for 1 hour; filter again after the gained filtrate stands for 2 hours, and then Combine the precipitates obtained by filtering twice, then wash and dry the combined precipitates; take the precipitates after washing and drying, add acetone equivalent to 15 times the mass of the precipitates, and then add dropwise at room temperature Dimethyl sulfate of 1.5 times the mass of the precipitate, then add NaOH powder equivalent to 0.5 times the mass of the precipitate, and then heat and reflux for 5 hours under stirring; after...

Embodiment 3

[0018] Get 50g of berberine, add dichloromethane equivalent to 10 times the quality of berberine, and stir to obtain system A; add anhydrous aluminum chloride equivalent to 2.5 times the quality of berberine to system A, and stir until the solid Then viscous and evenly dispersed into small particles, then sealed and placed for 24 hours, then add hydrochloric acid equivalent to 10 times the quality of berberine and a concentration of 6mol / L, filter after stirring for 1 hour; filter again after the gained filtrate stands for 2 hours, and then Combine the precipitates obtained by filtering twice, then wash and dry the combined precipitates; take the precipitates after washing and drying, add acetone equivalent to 15 times the mass of the precipitates, and then add dropwise at room temperature Dimethyl sulfate of 1.5 times the mass of the precipitate, then add NaOH powder equivalent to 0.5 times the mass of the precipitate, and then heat and reflux for 5 hours under stirring; after...

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PUM

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Abstract

The invention discloses a fibrauretine preparation method. The preparation method comprises the following steps: using berberine as a raw material, using methylene chloride as a solvent, using aluminium chloride to realize demethylation so as to obtain 5,6-dihydro-2,3,9,10-tetrahydroxy-dibenzo [a, g] quinolizine inner salt, and using methyl sulfate to realize methylation so as to obtain the fibrauretine with the yield of 60 percent and the purity of 91 percent. The method has the advantages of simple manufacturing process and simplicity and convenience in operation.

Description

technical field [0001] The invention belongs to the technical field of chemical medicine preparation and relates to a preparation method of palmatine. Background technique [0002] The chemical name of palmatine is 5,6-dihydro-2,3,9,10-tetramethoxydibenzo[a,g]quinazine ylide, which has a broad-spectrum antibacterial effect and can be used clinically to treat Gynecological inflammation, bacillary dysentery, enteritis, respiratory tract and urinary tract infection, surgical infection and conjunctivitis, etc. [0003] Lutein can be extracted and refined from the dried cane of Caulis Fibraurear, a plant of the family Fangjiceae, but resources are scarce and supply is in short supply. There are researches using 2-methoxyphenol as raw material to synthesize palmatine through methylation, chloromethylation, cyanation, hydroamination, condensation and cyclization, etc., but the preparation process is cumbersome. And the total yield is only about 10%. In another study, 5,6-dihydro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D455/03
Inventor 谭睿吴梅陈家渊
Owner SOUTHWEST JIAOTONG UNIV
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