CN102060756A - Method for preparing sodium picosulfate monohydrate - Google Patents
Method for preparing sodium picosulfate monohydrate Download PDFInfo
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- CN102060756A CN102060756A CN2010105539937A CN201010553993A CN102060756A CN 102060756 A CN102060756 A CN 102060756A CN 2010105539937 A CN2010105539937 A CN 2010105539937A CN 201010553993 A CN201010553993 A CN 201010553993A CN 102060756 A CN102060756 A CN 102060756A
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- sodium sulfate
- gram sodium
- sulfate monohydrate
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Abstract
The invention relates to a method for preparing sodium picosulfate monohydrate. The method is characterized by comprising the following steps of: dissolving sodium picosulfate anhydride in water-containing organic alcohol solution at the temperature of between 50 and 120 DEG C; filtering while the solution is hot; and standing filtrate at the temperature of between -20 and 70 DEG C and crystallizing, wherein a product is dried under vacuum at a constant temperature to prepare the sodium picosulfate monohydrate. Water content of the sodium picosulfate monohydrate is 3.6 to 3.8 percent; and both melting point and elemental analysis data meet the characteristics of the sodium picosulfate monohydrate.
Description
Technical field
The present invention relates to a preparation method of gram sodium sulfate monohydrate.
Background technology
Gram sodium sulfate (chemical name is: 4,4 '-(pyridine-2-methylene) two phenyl two sodium sulfovinates) is laxative commonly used clinically, and listing country comprises a plurality of countries such as Italy, Germany, Japan, Australia.Sodium picosulfate is the special laxative with unique effect mode, it becomes the diphenol metabolite by the metabolism of intestinal flora, this compound can make intestinal peristalsis hyperfunction, stimulate intestinal mucosa, reduce moisture absorption, thereby produce the catharsis effect, sodium picosulfate catharsis action temperature and, promote that defecation, operation front intestinal pipe content are got rid of, the preceding disposal of large intestine inspection (endoscopy), intestinal tube content eliminating etc. after being applicable to various constipations, the auxiliary defecation of postoperative, contrast medium administration.
Disclosed a gram Preparation of sodium method the earliest at patent GB1152199, it has disclosed 4,4 '-dihydroxyphenyl-(2-pyridine) methane and chlorsulfonic acid carry out esterification in the presence of pyridine, reaction solution obtains 4 through aftertreatment, the two sodium sulfovinates of 4 '-(pyridine-2-methylene) two phenyl.
What gram sodium sulfate was used clinically is the form of gram sodium sulfate monohydrate, but the gram Preparation of sodium method disclosed in the existing literature all is an anhydrous gram Preparation of sodium.
Mentioned 4 among the patent GB1152199,4 '-dihydroxyphenyl-(2-pyridine) methane and chlorsulfonic acid carry out esterification in the presence of pyridine, then reaction solution is poured in the water, neutralization reaction liquid, ether extraction is removed impurity, the solid dehydrated alcohol extraction that obtains behind the evaporated in vacuo water solvent directly obtains a gram sodium sulfate hydrate behind the evaporate to dryness ethanol.But, this invention is because with dehydrated alcohol extraction gram sodium sulfate crude product, in the solution that obtains water shortage forming the water content of a crystal water, and, directly solvent evaporated obtains a hydrate of gram sodium sulfate, and this process is unfavorable for forming a stable gram sodium sulfate monohydrate.The ultimate analysis data that it provides also are to match with anhydrous gram sodium sulfate.
Patent CH515902, ES543613, DE1904322, GB1345215 has prepared anhydrous gram sodium sulfate with US3528986 with identical method.Its fusing point that obtains, results of elemental analyses and anhydrous gram sodium sulfate match.
A patent GB1128736 dehydrated alcohol extraction gram sodium sulfate crude product, directly obtain a gram sodium sulfate hydrate behind the evaporate to dryness ethanol, but its gram sodium sulfate hydrate water content that obtains is far away from a water content ratio of gram sodium sulfate monohydrate 3.6% up to 6.5%.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of gram sodium sulfate monohydrate, a prepared gram sodium sulfate monohydrate is a white crystals, water absorbability is low, good stability.Product determines that through ultimate analysis, thermogravimetric analysis its water content is 3.6～3.8%.Resulting product quality meets European Pharmacopoeia, the desired quality standard of Japanese Pharmacopoeia.
The present invention realizes by following technical scheme:
1, molten sample: a gram sodium sulfate anhydride is dissolved in the organic alcoholic solution that contains water, and solvent temperature is 50 ~ 120 ℃;
2, crystallization: filtered while hot is removed a small amount of insoluble impurity in the solution, and filtrate is left standstill crystallization at-20 ~ 70 ℃;
3, drying: can obtain a gram sodium sulfate monohydrate after the product process vacuum constant temperature drying.
A gram sodium sulfate crude product of being mentioned is with reference to U.S. Pat 3528986 preparations, and concrete reaction process is seen formula 1:
Advantage of the present invention is a gram sodium sulfate monohydrate of (1) the present invention preparation, water content is 3.6～3.8%, fusing point, ultimate analysis data all meet a character of gram sodium sulfate monohydrate, and product quality meets European Pharmacopoeia, the desired quality standard of Japanese Pharmacopoeia; (2) the present invention adopts in the solution ratio of water excessive, makes that the content of water is enough to form a crystal water in the solution, and adopts in the crystallization process and leave standstill crystallization, compares with document in the past, more helps forming a stable gram sodium sulfate monohydrate.(3) provided by the invention gram sodium sulfate monohydrate preparation method, technology is simple, and is easy to operate, is fit to suitability for industrialized production.
Description of drawings:
Fig. 1 is the X-ray diffracting spectrum according to a gram sodium sulfate monohydrate of the present invention's gram sodium sulfate monohydrate preparation method preparation.
Fig. 2 is the TG collection of illustrative plates according to a gram sodium sulfate monohydrate of the present invention's gram sodium sulfate monohydrate preparation method preparation.
Embodiment:
Embodiment 1
Add the 50ml pure water in 600ml ethanol, a gram sodium sulfate crude product 60 gram can all dissolve during with this mixture heating up to 55 ~ 60 ℃, filtered while hot, and the filtrate that obtains is cooled to 20 ℃ and leaves standstill crystallization.The crystal that filtration is separated out with ice ethanol 20ml wash crystallization, 80 ℃ of decompression freeze-day with constant temperature, obtains gram sodium sulfate monohydrate 48.6 gram, and fusing point is 211.3 ~ 213.5 ℃.
Results of elemental analyses (C
18H
13NNa
2O
8S
2.H
2O): C, 43.15; H, 3.10; N, 2.76; Na, 9.17; S, 12.71
Theoretical value: C, 43.29; H, 3.03; N, 2.80; Na, 9.21; S, 12.84
Gram sodium sulfate anhydride theoretical value: C, 44.91; H, 2.72; N, 2.91; Na, 9.55; S, 13.32
Embodiment 2
Add the 57ml pure water in the 800ml Virahol, a gram sodium sulfate crude product 60 gram all dissolves during with this mixture heating up to 75 ~ 80 ℃, filtered while hot, and the filtrate that obtains is cooled to 20 ℃ and leaves standstill crystallization.The crystal that filtration is separated out with ice Virahol 30ml wash crystallization, 80 ℃ of decompression freeze-day with constant temperature, obtains gram sodium sulfate monohydrate 47.2 gram, and fusing point is 211.0 ~ 213.4 ℃.
Embodiment 3
Add the 57ml pure water in the 800ml n-propyl alcohol, a gram sodium sulfate crude product 60 gram all dissolves during with this mixture heating up to 83 ~ 86 ℃, filtered while hot, and the filtrate that obtains is cooled to 20 ℃ and leaves standstill crystallization.The crystal that filtration is separated out with ice Virahol 30ml wash crystallization, 80 ℃ of decompression freeze-day with constant temperature, obtains gram sodium sulfate monohydrate 47.5 gram, and fusing point is 210.9 ~ 213.7 ℃.
Embodiment 4
As embodiment 1, different is, and filtrate is cooled to 0 ℃ leaves standstill crystallization.Obtain gram sodium sulfate monohydrate 50.3 gram, fusing point is 209.5 ~ 213.2 ℃.
Embodiment 5
As embodiment 2, different is, and filtrate is cooled to 0 ℃ leaves standstill crystallization.Obtain gram sodium sulfate monohydrate 49.2 gram, fusing point is 210.0 ~ 213.1 ℃.
Claims (10)
1. the preparation method of a gram sodium sulfate monohydrate is characterized in that a gram sodium sulfate anhydride is dissolved in the organic alcoholic solution that contains water, and solvent temperature is 50 ~ 120 ℃, filters, and gained solution makes at-20 ~ 70 ℃ of crystallizatioies.
2. according to claim 1 gram sodium sulfate monohydrate preparation method is characterized in that a gram sodium sulfate anhydride is dissolved in the organic alcoholic solution that contains water, and the mass ratio of a gram sodium sulfate anhydride and water is 1: 0.1 ~ 3.0.
3. according to claim 2 gram sodium sulfate monohydrate preparation method is characterized in that the mass ratio of a gram sodium sulfate anhydride and water is 1: 0.6 ~ 1.4.
4. according to claim 1 gram sodium sulfate monohydrate preparation method, the organic alcoholic solution that it is characterized in that containing water is that water and alcohol are by 1: 2 ~ 40 mixed.
5. according to claim 4 gram sodium sulfate monohydrate preparation method, the organic alcoholic solution that it is characterized in that containing water is that water and alcohol are by 1: 10 ~ 15 mixed.
6. according to claim 1 gram sodium sulfate monohydrate preparation method is characterized in that alcoholic solution is organic alcoholic solutions such as ethanol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol.
7. according to claim 6 gram sodium sulfate monohydrate preparation method is characterized in that alcoholic solution is ethanol, n-propyl alcohol, Virahol.
8. according to claim 1 gram sodium sulfate monohydrate preparation method is characterized in that the solvent temperature scope is 50 ~ 120 ℃.
9. according to claim 1 gram sodium sulfate monohydrate preparation method is characterized in that crystalline range is-20 ~ 70 ℃.
10. according to claim 9 gram sodium sulfate monohydrate preparation method is characterized in that crystalline range is 0 ~ 30 ℃.
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| CN2010105539937A CN102060756B (en) | 2010-11-23 | 2010-11-23 | Method for preparing sodium picosulfate monohydrate |
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| CN2010105539937A CN102060756B (en) | 2010-11-23 | 2010-11-23 | Method for preparing sodium picosulfate monohydrate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114262110A (en) * | 2021-12-16 | 2022-04-01 | 湖南化工研究院有限公司 | Integrated synergic recovery method for sodium sulfate and methanol in wastewater from pirimiphos-methyl production |
| CN114957104A (en) * | 2022-06-17 | 2022-08-30 | 海南鑫开源医药科技有限公司 | Novel crystal form of sodium picosulfate monohydrate and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3686189A (en) * | 1966-12-14 | 1972-08-22 | Angeli Inst Spa | 3-halogenated 4,4'-disulfoxy-diphenyl-(2-pyridyl)-methane |
| WO2009007770A1 (en) * | 2007-07-06 | 2009-01-15 | Gumlink A/S | Chewing gum granules for compressed chewing gum |
-
2010
- 2010-11-23 CN CN2010105539937A patent/CN102060756B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3686189A (en) * | 1966-12-14 | 1972-08-22 | Angeli Inst Spa | 3-halogenated 4,4'-disulfoxy-diphenyl-(2-pyridyl)-methane |
| WO2009007770A1 (en) * | 2007-07-06 | 2009-01-15 | Gumlink A/S | Chewing gum granules for compressed chewing gum |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114262110A (en) * | 2021-12-16 | 2022-04-01 | 湖南化工研究院有限公司 | Integrated synergic recovery method for sodium sulfate and methanol in wastewater from pirimiphos-methyl production |
| CN114957104A (en) * | 2022-06-17 | 2022-08-30 | 海南鑫开源医药科技有限公司 | Novel crystal form of sodium picosulfate monohydrate and preparation method thereof |
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| CN102060756B (en) | 2013-03-13 |
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