CN1151154C - Preparation process of oxysophocarpine - Google Patents
Preparation process of oxysophocarpine Download PDFInfo
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- CN1151154C CN1151154C CNB001333518A CN00133351A CN1151154C CN 1151154 C CN1151154 C CN 1151154C CN B001333518 A CNB001333518 A CN B001333518A CN 00133351 A CN00133351 A CN 00133351A CN 1151154 C CN1151154 C CN 1151154C
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- sophocarpine
- preparation technology
- sophocarpidin
- extraction
- reaction solution
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- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The present invention provides a technology for preparing oxysophocarpine. Firstly, sophocarpine is added to hydrogen peroxide to react at a temperature of 25 to 90 DEG C; then, reaction liquid is extracted or concentrated by pressure reduction, and refluxed to obtain oxysophocarpine. The technology has the advantages of simplicity, practicability and high product yield, and is suitable for industrialized production.
Description
Technical field
The present invention relates to alkaloidal preparation, especially the preparation technology of Sophocarpidin.
Background technology
Sophocarpidin is one of natural alkaloid, does not still have the production technique of the Sophocarpidin that is suitable for suitability for industrialized production at present.
Summary of the invention
The purpose of this invention is to provide a kind of preparation technology who is suitable for the Sophocarpidin of suitability for industrialized production, features simple and practical process.
For achieving the above object, the present invention is by the following technical solutions:
The preparation technology of Sophocarpidin, concrete processing step is as follows:
(1) sophocarpine is added in the hydrogen peroxide;
(2) be 25-90 ℃ of scope internal reaction in temperature;
(3) reaction finishes, and the unreacted sophocarpine of a kind of extraction with in ethers, hydro carbons, the benzene class material does not have till the sophocarpine in reaction solution substantially;
(4) reaction solution concentrating under reduced pressure, a kind of extraction in decompressed concentrate haloalkane, the Ester, extraction liquid concentrating under reduced pressure, get medicinal extract, use the alcohols material dissolution filter again, filtrate decompression concentrates, add letones in the concentrated solution and reflux, cool off, separate out crystallization, suction filtration gets Sophocarpidin.
The preparation technology of Sophocarpidin, concrete processing step also can be:
(1) sophocarpine is added in the hydrogen peroxide;
(2) be 25-90 ℃ of scope internal reaction in temperature;
(3) reaction finishes, and the unreacted sophocarpine of a kind of extraction with in ethers, hydro carbons, the benzene class material does not have till the sophocarpine in reaction solution substantially;
(4) reaction solution concentrating under reduced pressure, decompressed concentrate adds the siccative drying with a kind of extraction in haloalkane, the Ester in the extraction liquid, filter, and adds ether material in the filtrate, separates out crystallization, is Sophocarpidin.
The preparation technology of Sophocarpidin, concrete processing step can also be:
(1) sophocarpine is added in the hydrogen peroxide;
(2) be 25-90 ℃ of scope internal reaction in temperature;
(3) reaction finishes, and the unreacted sophocarpine of a kind of extraction with in ethers, hydro carbons, the benzene class material does not have till the sophocarpine in reaction solution substantially;
(4) reaction solution concentrating under reduced pressure adds the alcohols material dissolving, suction filtration, and filtrate decompression concentrates, and adds letones and refluxes, and suction filtration obtains white crystals, is Sophocarpidin.
The preparation technology of Sophocarpidin, concrete processing step can also be:
(1) sophocarpine is added in the hydrogen peroxide;
(2) be 25-90 ℃ of scope internal reaction in temperature;
(3) reaction finishes, and the unreacted sophocarpine of a kind of extraction with in ethers, hydro carbons, the benzene class material does not have till the sophocarpine in reaction solution substantially;
(4) reaction solution concentrating under reduced pressure, decompressed concentrate adds ether material with a kind of extraction in haloalkane, the Ester in the extraction liquid, separate out white solid, is Sophocarpidin.
The present invention has following effect:
(1) processing method is simple and practical.
(2) product purity height.Calculate with dry product, products obtained therefrom purity can reach more than 98%.
(3) product yield height.
(4) processing method is suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1:
The 20g sophocarpine is joined in the 15g hydrogen peroxide, after 14 hours,, in reaction solution, do not have till the sophocarpine substantially with the unreacted sophocarpine of extracted with diethyl ether in 70 ℃ of reactions.With the reaction solution concentrating under reduced pressure, the decompressed concentrate chloroform extraction, the extraction liquid concentrating under reduced pressure gets medicinal extract, filter with dissolve with ethanol, filtrate decompression concentrates again, and adds acetone in the concentrated solution and refluxes, cools off, separates out crystallization, suction filtration obtains crystallization 15.5g, is Sophocarpidin.
Embodiment 2:
The 20g sophocarpine is joined in the 15g hydrogen peroxide,, extract unreacted sophocarpine, in reaction solution, do not have till the sophocarpine substantially with hexanaphthene in 60 ℃ of stirring reactions 14 hours.Behind the reaction solution concentrating under reduced pressure, use chloroform extraction, add anhydrous sodium sulfate drying in the extraction liquid and filter, add anhydrous diethyl ether in the filtrate, separate out crystallization 13g, be Sophocarpidin.
Embodiment 3:
The 100g sophocarpine is joined in the 75g hydrogen peroxide,, extract unreacted sophocarpine, in reaction solution, do not have till the sophocarpine substantially with benzene 40 ℃ of following stirring reactions 18 hours.With the reaction solution concentrating under reduced pressure, chloroform extraction adds anhydrous diethyl ether slowly in the chloroform solution, separate out white solid 90g, is Sophocarpidin.
Embodiment 4:
The 100g sophocarpine is joined in the 75g hydrogen peroxide,, extract unreacted sophocarpine, in reaction solution, do not have till the sophocarpine substantially with toluene 25 ℃ of following stirring reactions 18 hours.With the reaction solution concentrating under reduced pressure, add dissolve with ethanol, suction filtration, filtrate decompression concentrates, and adds acetone and refluxes, and suction filtration obtains white crystals 90g, is Sophocarpidin.
Embodiment 5:
The 100g sophocarpine is joined in the 75g hydrogen peroxide,,, in reaction solution, do not have till the sophocarpine substantially with the unreacted sophocarpine of xylene extraction 25 ℃ of following stirring reactions 18 hours.With the reaction solution concentrating under reduced pressure, add dissolve with ethanol, suction filtration, filtrate decompression concentrates, and adds acetone and refluxes, and suction filtration obtains white crystals 90g, is Sophocarpidin.
Chloroform among the above embodiment 1,2,3 can use ethylene dichloride, monochloroethane, methylene dichloride or tetracol phenixin to substitute.Also can change chloroform into ethyl acetate.Ether, sherwood oil, benzene,toluene,xylene, cyclohexane give are that extract can mutual alternative in above embodiment 1,2,3,4.
Claims (12)
1. the preparation technology of Sophocarpidin, concrete processing step is as follows:
(1) sophocarpine is added in the hydrogen peroxide;
(2) be 25-90 ℃ of scope internal reaction in temperature;
(3) reaction finishes, and the unreacted sophocarpine of a kind of extraction with in ethers, hydro carbons, the benzene class material does not have till the sophocarpine in reaction solution substantially;
(4) reaction solution concentrating under reduced pressure, a kind of extraction in decompressed concentrate haloalkane, the Ester, extraction liquid concentrating under reduced pressure, get medicinal extract, use the alcohols material dissolution filter again, filtrate decompression concentrates, add letones in the concentrated solution and reflux, cool off, separate out crystallization, suction filtration gets Sophocarpidin.
2. the preparation technology of Sophocarpidin, concrete processing step is as follows:
(1) sophocarpine is added in the hydrogen peroxide;
(2) be 25-90 ℃ of scope internal reaction in temperature;
(3) reaction finishes, and the unreacted sophocarpine of a kind of extraction with in ethers, hydro carbons, the benzene class material does not have till the sophocarpine in reaction solution substantially;
(4) reaction solution concentrating under reduced pressure, decompressed concentrate adds the siccative drying with a kind of extraction in haloalkane, the Ester in the extraction liquid, filter, and adds ether material in the filtrate, separates out crystallization, is Sophocarpidin.
3. the preparation technology of Sophocarpidin, concrete processing step is as follows:
(1) sophocarpine is added in the hydrogen peroxide;
(2) be 25-90 ℃ of scope internal reaction in temperature;
(3) reaction finishes, and the unreacted sophocarpine of a kind of extraction with in ethers, hydro carbons, the benzene class material does not have till the sophocarpine in reaction solution substantially;
(4) reaction solution concentrating under reduced pressure adds the alcohols material dissolving, suction filtration, and filtrate decompression concentrates, and adds letones and refluxes, and suction filtration obtains white crystals, is Sophocarpidin.
4. the preparation technology of Sophocarpidin, concrete processing step is as follows:
(1) sophocarpine is added in the hydrogen peroxide;
(2) be 25-90 ℃ of scope internal reaction in temperature;
(3) reaction finishes, and the unreacted sophocarpine of a kind of extraction with in ethers, hydro carbons, the benzene class material does not have till the sophocarpine in reaction solution substantially;
(4) reaction solution concentrating under reduced pressure, decompressed concentrate adds ether material with a kind of extraction in haloalkane, the Ester in the extraction liquid, separate out white solid, is Sophocarpidin.
5. as the preparation technology of claim 1 or 2 or 4 described Sophocarpidins, haloalkane is chloroform, ethylene dichloride, monochloroethane, methylene dichloride or tetracol phenixin.
6. as the preparation technology of claim 1 or 2 or 3 or 4 described Sophocarpidins, benzene class material is a benzene,toluene,xylene.
7. as the preparation technology of claim 1 or 2 or 3 or 4 described Sophocarpidins, ether material is ether, sherwood oil.
8. as the preparation technology of claim 1 or 3 described Sophocarpidins, alcohols material is an ethanol.
9. as the preparation technology of claim 1 or 2 or 4 described Sophocarpidins, Ester is an ethyl acetate.
10. as the preparation technology of claim 1 or 3 described Sophocarpidins, letones is an acetone.
11. the preparation technology of Sophocarpidin as claimed in claim 2, siccative is anhydrous sodium sulphate, Calcium Chloride Powder Anhydrous.
12., it is characterized in that described hydro carbons is a hexanaphthene as the preparation technology of claim 1 or 2 or 3 or 4 described Sophocarpidins.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001333518A CN1151154C (en) | 2000-11-18 | 2000-11-18 | Preparation process of oxysophocarpine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001333518A CN1151154C (en) | 2000-11-18 | 2000-11-18 | Preparation process of oxysophocarpine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1354181A CN1354181A (en) | 2002-06-19 |
| CN1151154C true CN1151154C (en) | 2004-05-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001333518A Expired - Fee Related CN1151154C (en) | 2000-11-18 | 2000-11-18 | Preparation process of oxysophocarpine |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100451019C (en) * | 2006-08-31 | 2009-01-14 | 中国医学科学院放射医学研究所 | Oxysophocarpine and its salt preparing method |
| CN102850352A (en) * | 2012-07-26 | 2013-01-02 | 宁夏紫荆花制药有限公司 | Preparation method high-purity high-yield oxysophocarpine |
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- 2000-11-18 CN CNB001333518A patent/CN1151154C/en not_active Expired - Fee Related
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| CN1354181A (en) | 2002-06-19 |
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Granted publication date: 20040526 Termination date: 20121118 |