CN104130253A - Anisodamine production method - Google Patents
Anisodamine production method Download PDFInfo
- Publication number
- CN104130253A CN104130253A CN201410306043.2A CN201410306043A CN104130253A CN 104130253 A CN104130253 A CN 104130253A CN 201410306043 A CN201410306043 A CN 201410306043A CN 104130253 A CN104130253 A CN 104130253A
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- CN
- China
- Prior art keywords
- anisodamine
- add
- chloroform
- production method
- carbon tetrachloride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D451/00—Heterocyclic compounds containing 8-azabicyclo [3.2.1] octane, 9-azabicyclo [3.3.1] nonane, or 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring systems, e.g. tropane or granatane alkaloids, scopolamine; Cyclic acetals thereof
- C07D451/02—Heterocyclic compounds containing 8-azabicyclo [3.2.1] octane, 9-azabicyclo [3.3.1] nonane, or 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring systems, e.g. tropane or granatane alkaloids, scopolamine; Cyclic acetals thereof containing not further condensed 8-azabicyclo [3.2.1] octane or 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring systems, e.g. tropane; Cyclic acetals thereof
- C07D451/04—Heterocyclic compounds containing 8-azabicyclo [3.2.1] octane, 9-azabicyclo [3.3.1] nonane, or 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring systems, e.g. tropane or granatane alkaloids, scopolamine; Cyclic acetals thereof containing not further condensed 8-azabicyclo [3.2.1] octane or 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring systems, e.g. tropane; Cyclic acetals thereof with hetero atoms directly attached in position 3 of the 8-azabicyclo [3.2.1] octane or in position 7 of the 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring system
- C07D451/06—Oxygen atoms
- C07D451/10—Oxygen atoms acylated by aliphatic or araliphatic carboxylic acids, e.g. atropine, scopolamine
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides an anisodamine production method which comprises the following steps: S1, taking belladonna coarse powder, adding 25% to 28% concentration of ammonia for soaking for 15-20min; S2, adding diethoxymethane for percolation, extracting the percolation liquid with 2% sulfuric acid; S3, adding chloroform for cleaning, adding the ammonia to adjust pH to 9, adding carbon tetrachloride for extraction; S4, adding water for washing carbon tetrachloride layer, and adding anhydrous sodium sulfate into chloroform layer for drying; S5, filtering and recovering the chloroform, adding anhydrous benzene for dissolution, and precipitating crystal; and S6, adding benzene for washing, drying at 55-60 DEG C to obtain anisodamine. The anisodamine production method improves the collection rate and collection purity of the anisodamine, the purity reaches 98%, and the process parameters are optimized.
Description
Technical field
The present invention relates to the production method of Anisodamine, be specifically related to utilize henbane meal to carry out a kind of production method of Anisodamine.
Background technology
Anisodamine anticholinergic drug.Can make smooth muscle loosening, remove vasospasm and therefore have analgesic effect, patent medicine has tablet and injection.Multiplex injection clinically, because of oral absorption poor.Anisodamine can be used for treatment and infects the diseases such as toxic shock, sciatica, gastric and duodenal ulcer, retinitis pigmentosa.Its chemical name is: (±)-6 β-Qiang Ji – 1 α H, 5 α H – Tuo Wan – 3 α – alcohol tropates.Chemical structural formula: molecular formula: C17H23NO4 molecular weight: 305.38.The method for making of current Anisodamine is because technique is coarse, and the collection ratio of Anisodamine is lower, causes a large amount of wastes.
Summary of the invention
The production method that the object of this invention is to provide a kind of Anisodamine, solves one or more problem in above-mentioned prior art.
Production method according to a kind of Anisodamine of the present invention, is characterized in that, comprises the steps:
S1, get henbane meal, add the ammoniacal liquor of 25%～28% concentration to soak, 15～20min;
S2, add methylene diethyl ether diacolation, percolate 2% sulphuric acid extraction;
S3, add chloroform to clean, add ammoniacal liquor to adjust pH to refer to be 9, add carbon tetrachloride extraction.
S4, add water to clean carbon tetrachloride layer, chloroform layer adds anhydrous sodium sulfate drying;
S5, filtered and recycled chloroform, add dry-out benzene to dissolve, crystallization;
S6, add benzene washing, 55～60 ℃ dry, obtain Anisodamine.
Collection rate of the present invention has improved the collection purity of Anisodamine, and purity reaches 98%.
Embodiment
Embodiment 1:
The production method that the invention provides a kind of Anisodamine, is characterized in that, comprises the steps:
S1, get henbane meal, add the ammoniacal liquor of 25% concentration to soak, 15min;
S2, add methylene diethyl ether diacolation, percolate 2% sulphuric acid extraction;
S3, add chloroform to clean, add ammoniacal liquor to adjust pH to refer to be 8, add carbon tetrachloride extraction.
S4, add water to clean carbon tetrachloride layer, be adjusted to pH value 9; With chloroform extraction, chloroform layer adds anhydrous sodium sulfate drying;
S5, filtered and recycled chloroform, residue adds dry-out benzene to dissolve, crystallization;
S6, add benzene washing, 55 ℃ dry, obtain Anisodamine.
Collection rate of the present invention has improved the collection purity of Anisodamine, and purity reaches 95%.
Embodiment 2:
The production method that the invention provides a kind of Anisodamine, is characterized in that, comprises the steps:
S1, get henbane meal, add the ammoniacal liquor of 26.5% concentration to soak, 17min;
S2, add methylene diethyl ether diacolation, percolate 2% sulphuric acid extraction;
S3, add chloroform to clean, add ammoniacal liquor to adjust pH to refer to be 8, add carbon tetrachloride extraction.
S4, add water to clean carbon tetrachloride layer, be adjusted to pH value 9.5; With chloroform extraction, chloroform layer adds anhydrous sodium sulfate drying;
S5, filtered and recycled chloroform, residue adds dry-out benzene to dissolve, crystallization;
S6, add benzene washing, 57 ℃ dry, obtain Anisodamine.
Collection rate of the present invention has improved the collection purity of Anisodamine, and purity reaches 97%.
Embodiment 3:
The production method that the invention provides a kind of Anisodamine, is characterized in that, comprises the steps:
S1, get henbane meal, add the ammoniacal liquor of 28% concentration to soak, 20min;
S2, add methylene diethyl ether diacolation, percolate 2% sulphuric acid extraction;
S3, add chloroform to clean, add ammoniacal liquor to adjust pH to refer to be 9, add carbon tetrachloride extraction.
S4, add water to clean carbon tetrachloride layer, be adjusted to pH value 10; With chloroform extraction, chloroform layer adds anhydrous sodium sulfate drying;
S5, filtered and recycled chloroform, residue adds dry-out benzene to dissolve, crystallization;
S6, add benzene washing, 60 ℃ dry, obtain Anisodamine.
Collection rate of the present invention has improved the collection purity of Anisodamine, and purity reaches 98%.
More than statement is only optimal way of the present invention, it should be pointed out that to those skilled in the art, without departing from the concept of the premise of the invention, can also make some distortion and improvement, within these also should be considered as protection scope of the present invention.
Claims (2)
1. a production method for Anisodamine, is characterized in that, comprises the steps:
S1, get henbane meal, add the ammoniacal liquor of 25%～28% concentration to soak, 15～20min;
S2, add methylene diethyl ether diacolation, percolate 2% sulphuric acid extraction;
S3, add chloroform to clean, add ammoniacal liquor to adjust pH to refer to be 9, add carbon tetrachloride extraction.
2. the production method of a kind of Anisodamine according to claim 1, is characterized in that, also comprises the following steps after S3:
S4, add water to clean carbon tetrachloride layer, chloroform layer adds anhydrous sodium sulfate drying;
S5, filtered and recycled chloroform, add dry-out benzene to dissolve, crystallization;
S6, add benzene washing, 55～60 ℃ dry, obtain Anisodamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410306043.2A CN104130253A (en) | 2014-06-30 | 2014-06-30 | Anisodamine production method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410306043.2A CN104130253A (en) | 2014-06-30 | 2014-06-30 | Anisodamine production method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104130253A true CN104130253A (en) | 2014-11-05 |
Family
ID=51803145
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410306043.2A Pending CN104130253A (en) | 2014-06-30 | 2014-06-30 | Anisodamine production method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104130253A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674217A (en) * | 2016-12-15 | 2017-05-17 | 杭州民生药业有限公司 | Racanisodamine crystal form and preparation method thereof |
| CN113527286A (en) * | 2021-08-31 | 2021-10-22 | 锦州拾正生物科技有限公司 | Method for separating and purifying anisodamine monomer from alkaloid leaching paste |
| CN113698397A (en) * | 2021-08-28 | 2021-11-26 | 锦州拾正生物科技有限公司 | Anisodamine and purification process thereof |
| CN114276342A (en) * | 2021-12-29 | 2022-04-05 | 锦州拾正生物科技有限公司 | Method for separating and purifying anisodamine monomer from plant extract |
| CN116676355A (en) * | 2023-08-03 | 2023-09-01 | 成都第一制药有限公司 | Method for catalytic synthesis of anisodamine |
-
2014
- 2014-06-30 CN CN201410306043.2A patent/CN104130253A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 孙文基主编: "《天然药物成分提取分离与制备》", 30 November 1999 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674217A (en) * | 2016-12-15 | 2017-05-17 | 杭州民生药业有限公司 | Racanisodamine crystal form and preparation method thereof |
| CN106674217B (en) * | 2016-12-15 | 2019-02-05 | 杭州民生药业有限公司 | Racanisodamine crystal form and preparation method thereof |
| CN113698397A (en) * | 2021-08-28 | 2021-11-26 | 锦州拾正生物科技有限公司 | Anisodamine and purification process thereof |
| CN113527286A (en) * | 2021-08-31 | 2021-10-22 | 锦州拾正生物科技有限公司 | Method for separating and purifying anisodamine monomer from alkaloid leaching paste |
| CN114276342A (en) * | 2021-12-29 | 2022-04-05 | 锦州拾正生物科技有限公司 | Method for separating and purifying anisodamine monomer from plant extract |
| CN116676355A (en) * | 2023-08-03 | 2023-09-01 | 成都第一制药有限公司 | Method for catalytic synthesis of anisodamine |
| CN116676355B (en) * | 2023-08-03 | 2023-10-24 | 成都第一制药有限公司 | Method for catalytic synthesis of anisodamine |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20141105 |