CN1473829A - Process for preparing oxymatrine - Google Patents

Process for preparing oxymatrine Download PDF

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Publication number
CN1473829A
CN1473829A CNA031370489A CN03137048A CN1473829A CN 1473829 A CN1473829 A CN 1473829A CN A031370489 A CNA031370489 A CN A031370489A CN 03137048 A CN03137048 A CN 03137048A CN 1473829 A CN1473829 A CN 1473829A
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CN
China
Prior art keywords
oxymatyine
matrine
oxymatrine
hydrogen peroxide
preparing
Prior art date
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Pending
Application number
CNA031370489A
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Chinese (zh)
Inventor
平 刘
刘平
姜宏英
沈美丽
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Individual
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Individual
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Publication date
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Priority to CNA031370489A priority Critical patent/CN1473829A/en
Publication of CN1473829A publication Critical patent/CN1473829A/en
Pending legal-status Critical Current

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Abstract

The process of preparing oxymatrine is to oxidize matrine with hydrogen peroxide. The present invention has the advantages of rich material source, simple technological process and low toxicity of the product. The prepared oxymatrine as one medicinal material has the functions of killing bacteria, diminishing inflammation, resisting virus and resisting cancer.

Description

The preparation method of Oxymatyine
Technical field
The present invention relates to the preparation method of nitrogen-containing heterocycle compound, particularly relate to the preparation method of Oxymatyine.
Background technology
Oxymatyine is present in the root of leguminous plants kuh-seng, root has sand fixation, from natural leguminous plants, extract, can destroy the ecotope of the Nature, in addition, the Oxymatyine drug toxicity is lower than matrine, and has antitoxin anti-inflammatory, antiviral, anticancer effect, therefore, be badly in need of exploitation Oxymatyine product and become the task of top priority.
Summary of the invention:
The objective of the invention is to overcome the deficiencies in the prior art part, and provide a kind of method uncomplicated, the preparation method of effective Oxymatyine.
The present invention seeks to realize by following measure: the preparation method of Oxymatyine is that matrine is water-soluble, add 30% hydrogen peroxide, matrine and hydrogen peroxide weight ratio are 1: 3~4, hydro-oxidation sodium, PH7.2~7.8, heat 30~80 ℃, concentrate ethylene dichloride distillation, toluene recrystallization, drying makes white Oxymatyine product.
The molecular formula of matrine and Oxymatyine and structural formula, division is as follows
Title molecular formula mp (c)
Matrine matrine C 15H 24N 2O 74-76 ℃
Oxymatyine oxymatine C 15H 24N 2O 2214 ℃
Figure A0313704800032
The present invention has following advantage compared to existing technology: because matrine LD 50Be 300 milligrams/kilogram, and Oxymatyine LD 50It is 988 milligrams/kilogram, the toxicity that Oxymatyine is described is lower than matrine, matrine is externally applied agent in addition, reaction is big, and Oxymatyine is a medicine for oral administration, and is little to the patient reaction, State Drug Administration's official approval Oxymatyine is the bulk drug of traditional Chinese medicines, abundant because of raw material sources of the present invention again, prepare uncomplicatedly, have exploitation value.
EmbodimentEnumerating an embodiment is below further specified the present invention.
Embodiment 1 concrete preparation method:
1, soluble in water the matrine crystal, add 30% hydrogen peroxide, carry out oxidizing reaction, by weight, proportioning is H 2O 2: matrine 3-4: 1, differentiate no matrine spot until reactant through TLC.
2, use 20% caustic lye of soda, transfer PH7.2~7.8, heat 30~80 ℃, the hydrogen peroxide of decomposing excessive behind the concentrating under reduced pressure, is removed most of moisture, adds matrine weight 5-7 ethylene dichloride doubly again, boils distillation, removes residual moisture, filters.
3, filtrate distillation, concentrated, make filtrate volume be matrine 3-4 doubly, add 1: 1.5 toluene again, boil off partial solvent after the heating for dissolving, naturally cooling occurs until the Oxymatyine crystallization, and toluene wash 2-3 time used in the centrifugation crystallization, vacuum-drying promptly obtains the product of Oxymatyine of white.
Oxymatyine of the present invention adopts the thin-layer chromatography method to measure, and its method is as follows:
Get test specimen an amount of (about 50mg), add dehydrated alcohol, shake up and do trial-product to 25ml.Other gets the Oxymatyine standard substance, adds dehydrated alcohol, makes the solution that every 1ml contains 2mg and makees reference substance.Test and get each 20 microlitre of above-mentioned two kinds of samples according to tlc, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-liquor ammoniae fortis (5: 0.6: 0.3) is that developping agent launches, taking-up is dried spray and is developed the color with rare bismuth potassium iodide test solution, the color and the position of the principal spot that need testing solution shows, should be identical with the reference substance solution principal spot, other spot that do not have occurs.
Product of the present invention has antitoxin anti-inflammatory, and is antiviral, anticancer effect.

Claims (1)

1, the preparation method of Oxymatyine, it is characterized in that matrine water-soluble, add 30% hydrogen peroxide, matrine and hydrogen peroxide weight ratio are 1: 3~4, hydro-oxidation sodium, PH7.2~7.8, heat 30~80 ℃, concentrate, the ethylene dichloride distillation, the toluene recrystallization makes white Oxymatyine product.
CNA031370489A 2003-06-02 2003-06-02 Process for preparing oxymatrine Pending CN1473829A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNA031370489A CN1473829A (en) 2003-06-02 2003-06-02 Process for preparing oxymatrine

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNA031370489A CN1473829A (en) 2003-06-02 2003-06-02 Process for preparing oxymatrine

Publications (1)

Publication Number Publication Date
CN1473829A true CN1473829A (en) 2004-02-11

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Family Applications (1)

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CNA031370489A Pending CN1473829A (en) 2003-06-02 2003-06-02 Process for preparing oxymatrine

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CN (1) CN1473829A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102285987A (en) * 2011-08-15 2011-12-21 江苏天晟药业有限公司 Novel preparation process of oxymatrine

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102285987A (en) * 2011-08-15 2011-12-21 江苏天晟药业有限公司 Novel preparation process of oxymatrine

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