CN101195619B - Novel method for fine purification of theobromine - Google Patents
Novel method for fine purification of theobromine Download PDFInfo
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- CN101195619B CN101195619B CN2007101160008A CN200710116000A CN101195619B CN 101195619 B CN101195619 B CN 101195619B CN 2007101160008 A CN2007101160008 A CN 2007101160008A CN 200710116000 A CN200710116000 A CN 200710116000A CN 101195619 B CN101195619 B CN 101195619B
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- theobromine
- reductive agent
- crude product
- santheose
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Abstract
The invention relates to a refining method of santheose, which is characterized in that dissolves liquid alkali into crude santheose solution, decolourizes, fitlers, and adds reduction agent into filter liquor, acidifies at 60-80DEG C until pH=1-5, filters and dries to obtain santheose final product. The inventive method has refining yield of 90%, standard product color, high product quality, lowcost and industrialization suitability.
Description
Technical field
The invention belongs to the process for purification of Chemicals, particularly the process for purification of Theobromine.
Background technology
Theobromine (English name: Theobromine, 3,7-dimethyl-3,7-dihydro-1H-purine-2, the 6-diketone) is the central nervous stimulant of xanthine, the Theobromine crude product is essential refining by alkali (30% sodium hydroxide) earlier in the existing technology, carries out the solution color and luster after the acid treating again and just can meet the finished product standard.Twice refining, and refining rate is low.In addition, because sulfuric acid has certain destructiveness, lost a part of Theobromine, cost is higher, and production has been produced adverse influence.
Summary of the invention
The simple method that the purpose of this invention is to provide a kind of cacao preparate alkali that suitability for industrialized production value is more arranged, finished product color and luster conformance with standard, refining yield height.
A kind of Theobromine purified of the present invention novel method is characterized in that: Theobromine crude product solution liquid feeding alkali dissolution, decolouring is filtered, and adds reductive agent in the filtrate, and in 60～80 ℃ of acidifyings, filter acidifying terminal point PH=5～6, the dry Theobromine finished product that gets.
Described reductive agent is selected S-WAT, sodium bisulfite, Sodium Pyrosulfite, sodium sulphite, Sulfothiorine or hydrogen sulfide etc.
Optimized technical scheme is:
The weight ratio of Theobromine crude product and reductive agent is 1: 0.01～0.03.
By weight, Theobromine: 30% liquid caustic soda: reductive agent=1: 0.75: 0.01～0.03.
Souring temperature is 65～70 ℃.
In the Theobromine crude product, add concentration and be after 30% sodium hydroxide becomes the sodium salt dissolving, color is dark-brown, reason is that the oxidized color and luster that makes of some Theobromine darkens, add a spot of reductive agent, at a certain temperature, acidifying simultaneously, the oxidized Theobromine of a part is reduced and has generated Theobromine, dull the color, be generally light yellow, finished product color and luster conformance with standard; Make with extra care yield up to 90%, good product quality, low, the very suitable industrialized production of cost.
Embodiment
Embodiment 1:
In having the 250ml four-hole reaction flask of stirring, add Theobromine crude product 20 grams, add water 120ml, 30% liquid caustic soda 12ml, be warmed up to 70～80 ℃ under stirring, add gac 1 gram.Under this temperature, decolour half an hour.Filter, add Sodium Pyrosulfite 0.2 in the filtrate and restrain, stir and cool to 70 ℃, keep 65～70 ℃, be acidified to PH:5～6, cool to 25 ℃, filter with concentrated hydrochloric acid, qualified with deionized water wash, dry that Theobromine finished product 18.5 restrains to chlorion.It is qualified to examine entirely by cp2005, EP4, USP27.
Embodiment 2:
In having the 250ml four-hole reaction flask of stirring, add Theobromine crude product 20 grams, add water 120ml, 30% liquid caustic soda 12ml, be warmed up to 70～80 ℃ under stirring, add gac 1 gram.Under this temperature, decolour half an hour.Filter, add sodium bisulfite 0.3 in the filtrate and restrain, stir and cool to 70 ℃, keep 65～70 ℃, be acidified to PH:5～6, cool to 25 ℃, filter with concentrated hydrochloric acid, qualified with deionized water wash, dry that Theobromine finished product 18.6 restrains to chlorion.It is qualified to examine entirely by cp2005, EP4, USP27.
Embodiment 3:
In having the 250ml four-hole reaction flask of stirring, add Theobromine crude product 20 grams, add water 120ml, 30% liquid caustic soda 12ml, be warmed up to 70～80 ℃ under stirring, add gac 1 gram.Under this temperature, decolour half an hour.Filter, add Sulfothiorine 0.4 in the filtrate and restrain, stir and cool to 70 ℃, keep 65～70 ℃, be acidified to PH:5～6, cool to 25 ℃, filter with concentrated hydrochloric acid, qualified with deionized water wash, dry that Theobromine finished product 18.2 restrains to chlorion.It is qualified to examine entirely by cp2005, EP4, USP27.
Claims (3)
1. Theobromine purified method is characterized in that: Theobromine crude product solution liquid feeding alkali dissolution, and decolouring is filtered, and adds reductive agent in the filtrate, and in 60～80 ℃ of acidifyings, filter acidifying terminal point PH=5～6, dry Theobromine finished product; Wherein said reductive agent is S-WAT, sodium bisulfite, Sodium Pyrosulfite, sodium sulphite, Sulfothiorine or hydrogen sulfide.
2. Theobromine purified method according to claim 1 is characterized in that: the weight ratio of Theobromine crude product and reductive agent is 1: 0.01～0.03.
3. Theobromine purified method according to claim 1 is characterized in that: described liquid caustic soda is that concentration is 30% solution, by weight, and Theobromine: liquid caustic soda: reductive agent=1: 0.75: 0.01～0.03.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101160008A CN101195619B (en) | 2007-12-14 | 2007-12-14 | Novel method for fine purification of theobromine |
| CN200880121060.1A CN101896484B (en) | 2007-12-14 | 2008-12-12 | Theobromine production process |
| PCT/CN2008/001998 WO2009089677A1 (en) | 2007-12-14 | 2008-12-12 | Theobromine production process |
| IL206338A IL206338A0 (en) | 2007-12-14 | 2010-06-13 | Theobromine production process |
| IL227837A IL227837A0 (en) | 2007-12-14 | 2013-08-06 | Theobromine production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101160008A CN101195619B (en) | 2007-12-14 | 2007-12-14 | Novel method for fine purification of theobromine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101195619A CN101195619A (en) | 2008-06-11 |
| CN101195619B true CN101195619B (en) | 2010-12-08 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101160008A Expired - Fee Related CN101195619B (en) | 2007-12-14 | 2007-12-14 | Novel method for fine purification of theobromine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101195619B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108164530A (en) * | 2018-01-24 | 2018-06-15 | 安徽省百花香料香精有限公司 | A kind of environmentally friendly process for purification of theobromine |
| CN109503585B (en) * | 2018-12-29 | 2021-05-14 | 石药集团新诺威制药股份有限公司 | Refining method of pentoxifylline recovered product |
| CN114478530B (en) * | 2022-02-25 | 2023-09-19 | 陕西嘉禾药业有限公司 | Method for extracting high-content theobromine from cocoa beans |
| CN117304190A (en) * | 2023-11-29 | 2023-12-29 | 广州市桐晖药业有限公司 | Method for preparing pentoxifylline |
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2007
- 2007-12-14 CN CN2007101160008A patent/CN101195619B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101195619A (en) | 2008-06-11 |
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| PB01 | Publication | ||
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| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20090109 Address after: Shanghai City, Beijing Road No. 1701 Jingan China Mansion No. 200040: 28092810 post encoding Applicant after: Bailigao Trade (Shanghai)Co., Ltd. Address before: The postcode of Zibo hi tech Industrial Development Zone, Shandong Province, China: 255000 Applicant before: Shandong Xinhua Pharmaceutical Co., Ltd. |
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| ASS | Succession or assignment of patent right |
Owner name: BAILIGAO TRADE( SHANGHAI ) CO., LTD. Free format text: FORMER OWNER: SHANDONG XINHUA PHARMACY STOCK CO., LTD. Effective date: 20090109 |
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Granted publication date: 20101208 Termination date: 20131214 |