CN101037406B - Synthesizing method of garlic oil - Google Patents
Synthesizing method of garlic oil Download PDFInfo
- Publication number
- CN101037406B CN101037406B CN200610057594A CN200610057594A CN101037406B CN 101037406 B CN101037406 B CN 101037406B CN 200610057594 A CN200610057594 A CN 200610057594A CN 200610057594 A CN200610057594 A CN 200610057594A CN 101037406 B CN101037406 B CN 101037406B
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- CN
- China
- Prior art keywords
- bulbus allii
- oleum bulbus
- garlic oil
- reaction
- organic solvent
- 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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention relates to a synthesis method of the garlic oil, including making a replacement reaction with sodium sulfide and chloropropene in the organic solvent so as to precipitate sodium chloride; doing a sulfuration reaction by simple substance sulfur, then distilling to get the garlic oil. The product quality can attain the official standards of medicine, hygienic standard of food and Hygienic standard of feed.
Description
Technical field
The invention belongs to medicine, foodstuff additive and feed additive field, is the synthetic method of Oleum Bulbus Allii (Alltride).
The main effective constituent of Oleum Bulbus Allii is diallyl trithioether (CH
2=CH-CH
2-S-S-S-CH
2-CH=CH
2).
Background technology
Oleum Bulbus Allii has another name called garlic vegetable oil or garlicin, and special garlic taste is arranged, and can prevent and treat multiple transmissible disease, is a kind of broad spectrum antibiotic.Have multiple very strong biological function, as anti-cancer, blood pressure regulation, be good for the stomach, antiviral etc.Oleum Bulbus Allii unique biological characteristic does not have antibiotic side effect for having antibiotic effect, does not find organizing medium-term and long-term residual phenomena yet.Now be widely used in medicine, veterinary drug, agricultural chemicals and the foodstuff additive.
There are two kinds of natural extract and chemosynthesis in the source of Oleum Bulbus Allii, and the Oleum Bulbus Allii of natural extract limits it and is extensive use of owing to being subjected to starting material influence in short supply, factor such as yield poorly.Aspect chemosynthesis, narrated a kind of synthetic method of Oleum Bulbus Allii as domestic patent CN88105457.7, adopt Sulfothiorine, sodium sulphite and propenyl chloride to do raw material, there is long reaction time in this method, and yield is low, and shortcomings such as sewage discharge are arranged.Simultaneously, Oleum Bulbus Allii is in alkalescence and have under the condition that water exists unstablely, easily takes place to decompose and side reaction, and this production technique reaction times is at 6～8h, side reaction in the buffered soln of water medium, has taken place in reaction product for a long time, causes the decline of finished product Oleum Bulbus Allii yield.
The invention provides a new synthetic route, shortened the reaction times, reduced production cost, improve product yield, use the organic solvent of reusable edible simultaneously, solved the problem of sewage discharge in the production process.
Summary of the invention
The object of the invention is to overcome the deficiency of existing synthetic technology, and the feasible Oleum Bulbus Allii industrialized process for preparing of easy, a high yield of cover and without sewage discharge is provided.
The present invention is with sodium sulphite and propenyl chloride in organic solvent replacement(metathesis)reaction takes place and precipitated sodium chloride carries out vulcanization reaction with elemental sulfur, and then through distilling out Oleum Bulbus Allii, quality product reaches the national drug standards, food hygienic standard and forage health standard.
Building-up reactions formula of the present invention is as follows:
Na
2S+CH
2＝CH-CH
2-Cl+S→CH
2＝CH
2-CH
2-S-S-S-CH
2-CH＝CH
2+NaCl
Above-mentioned reaction preferably is controlled at 40～60 ℃, reaction times 2～3h, yield 95～98%, need not make water in the whole process of production, employed organic solvent reclaims through distillation and can be recycled, and whole process of production does not have sewage emissions, has solved many environmental issues.
Above-mentioned reaction conditions organic solvent can be ethanol, tetracol phenixin etc.
Production technique of the present invention is carried out in organic solvent, need not acid or alkali buffered soln, operational safety.
Specifically, the synthetic method of a kind of Oleum Bulbus Allii that the present invention relates to is characterized in that with elemental sulfur, sodium sulphite and propenyl chloride one-step synthesis Oleum Bulbus Allii in organic solvent, and need not with acid or alkali buffered soln, production process without sewage discharge.
Specific examples
With 95% ethanol (107g), 63.5% sodium sulphite (68.7g), 98% propenyl chloride (38.3g), 99% SULPHUR POWDER (17.5g) places three mouthfuls of round-bottomed flasks of 500ml, magnetic agitation, the empty packet temperature is in 48～53 ℃, backflow 3h, reaction is finished, cooling, the precipitated sodium chloride crystal filters, and filtrate is through underpressure distillation, reclaim the first cut alcohol solvent earlier, collecting the light yellow oily liquid of second cut then is Oleum Bulbus Allii (43.3g), yield 97.2%, content 99.2%{ national drug standards WS-10001-(HD-0500)-2002}, relative density (20/25 ℃) 1.104～1.110, refractive index (20 ℃): 1.585～1.590.
Claims (2)
1. the synthetic method of an Oleum Bulbus Allii is characterized in that with elemental sulfur, sodium sulphite and propenyl chloride one-step synthesis Oleum Bulbus Allii in organic solvent.
2. the synthetic method described in claim 1 is characterized in that need not with acid or alkali buffered soln, production process without sewage discharge.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610057594A CN101037406B (en) | 2006-03-16 | 2006-03-16 | Synthesizing method of garlic oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610057594A CN101037406B (en) | 2006-03-16 | 2006-03-16 | Synthesizing method of garlic oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101037406A CN101037406A (en) | 2007-09-19 |
| CN101037406B true CN101037406B (en) | 2010-05-12 |
Family
ID=38888611
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200610057594A Expired - Fee Related CN101037406B (en) | 2006-03-16 | 2006-03-16 | Synthesizing method of garlic oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101037406B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693576A (en) * | 2016-03-30 | 2016-06-22 | 洛阳和梦科技有限公司 | Preparation method of diallyl polythioether compounds |
| CN106588730B (en) * | 2016-12-02 | 2019-01-11 | 山东吉田香料股份有限公司 | A kind of preparation method of Diallytrisin |
| CN107188838A (en) * | 2017-06-21 | 2017-09-22 | 宜兴市天石饲料有限公司 | A kind of processing method of garlic oil |
| CN112294780A (en) * | 2020-10-15 | 2021-02-02 | 苏州大学 | Modulators, test methods and uses for modulating angiotensin-converting enzyme 2 activity |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006016881A1 (en) * | 2004-07-09 | 2006-02-16 | Albemarle Corporation | Process for producing diallyl disulfide |
-
2006
- 2006-03-16 CN CN200610057594A patent/CN101037406B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006016881A1 (en) * | 2004-07-09 | 2006-02-16 | Albemarle Corporation | Process for producing diallyl disulfide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101037406A (en) | 2007-09-19 |
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| DD01 | Delivery of document by public notice |
Addressee: Chen Peiqiao Document name: Written notice of preliminary examination of application for patent for invention |
|
| C06 | Publication | ||
| PB01 | Publication | ||
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| DD01 | Delivery of document by public notice |
Addressee: Chen Peiqiao Document name: Notice of publication of application for patent for invention |
|
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| ASS | Succession or assignment of patent right |
Owner name: BEIJING ZIYUAN ASIA PACIFIC FODDER SCIENCE CO., LT Free format text: FORMER OWNER: BEIJING ZIYUAN ASIA PACIFIC ANIMAL MEDICAL CO., LTD. Effective date: 20090731 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20090731 Address after: Huang Xing Zheng Village Daxing District street Beijing city science and technology No. 31 building eight layer encoding post: 102600 Applicant after: Beijing Resource Asia-Pacific Feed Technology Co., Ltd. Address before: Beijing city Daxing District yufazhen this Rong Street No. 98 post encoding: 102600 Applicant before: Beijing Resource Yatai Animal Medicine Co., Ltd. |
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Addressee: Beijing Resource Asia-Pacific Feed Technology Co., Ltd. Chen Peiqiao Document name: Notification to Pay the Fees |
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Addressee: Beijing Resource Asia-Pacific Feed Technology Co., Ltd. Document name: Notification of Decision on Request for Restoration of Right |
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Effective date of registration: 20160324 Address after: 410600 No. 2 resource Avenue, Ningxiang Economic Development Zone, Changsha, Hunan Patentee after: Hunan modern resources biotechnology Co Ltd Address before: 102600 Beijing city Daxing District Huangcun Xing Zheng Street No. 31 building eight layer technology Patentee before: Beijing Resource Asia-Pacific Feed Technology Co., Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee |
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| CF01 | Termination of patent right due to non-payment of annual fee |