CN103910685A - Method used for purifying sulfadimoxine - Google Patents
Method used for purifying sulfadimoxine Download PDFInfo
- Publication number
- CN103910685A CN103910685A CN201410083160.7A CN201410083160A CN103910685A CN 103910685 A CN103910685 A CN 103910685A CN 201410083160 A CN201410083160 A CN 201410083160A CN 103910685 A CN103910685 A CN 103910685A
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- CN
- China
- Prior art keywords
- sulphormethoxine
- filtrate
- acid solution
- sulfadimoxine
- acetic acid
- 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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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
- C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
- C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
- C07D239/69—Benzenesulfonamido-pyrimidines
Abstract
The invention relates to a method used for purifying sulfadimoxine. The method comprises following steps: (a) deionized water and calcium hydrate are delivered into a reaction container, an obtained mixture is heated to 80 to 85 DEG C, a sulfadimoxine coarse product is added with stirring, and pH value is adjusted to 9.5 to 10.5 so as to realize complete dissolving; (b) active carbon is delivered into the reaction container, an obtained mixed material is stirred for 0.5 to 2h at a temperature of 80 to 85 DEG C, and a filtrate is obtained via filtration; and (c) gracial acetate acid solution is added dropwise into the filtrate at a temperature of 75 to 80 DEG C, and then an obtained material is cooled via ice-water bath, pH value is adjusted to 5.1 to 5.4, the material is allowed to stand, and is subjected to centrifugal dewatering after precipitation, and a filter residue is collected. According to the method, gracial acetate acid solution is added dropwise into the filtrate, the obtained material is allowed to stand for precipitation, and is cooled via ice-water bath, so that sulfadimoxine can be precipitated rapidly, influences caused by other impurities are avoided, and purity and yield of sulfadimoxine are increased.
Description
Technical field
The present invention relates to a kind of preparation method of sulphormethoxine, be specifically related to a kind of method of the sulphormethoxine of purifying.
Background technology
Sulphormethoxine, chemistry 4-(p-amino benzene sulfonyl)-5 by name, 6-dimethoxypyridin, be generally used for the treatment of inflammation, as upper respiratory tract infection tonsillitis, bacillary dysentery enteritis, skin infections etc., also can coordinate with other drug, be used for the treatment of pulmonary tuberculosis, lymphoid tuberculosis.Sulphormethoxine has experienced several generations' research and development, and its production technique is progressively stable, is specially following preparation process:
Step (1):
Step (2):
Step (3):
Step (4):
Step (5):
Granted publication number is the method for purification that the Chinese invention patent of CN102304095B discloses a kind of sulphormethoxine, utilizes and adds respectively the adjusting such as calcium hydroxide, Glacial acetic acid pH that it is separated out in sulphormethoxine solution.Although aforesaid method can improve the purity of sulphormethoxine, be wherein still mixed with more impurity.For medicine intermediate field, its purity requirement to sulphormethoxine is higher, otherwise people is known from experience and produces immeasurable impact.
Summary of the invention
The present invention seeks to provide in order to overcome the deficiencies in the prior art a kind of method of the sulphormethoxine of purifying.
For achieving the above object, the technical solution used in the present invention is: a kind of method of the sulphormethoxine of purifying, comprise the following steps successively,
(a) in reaction vessel, add deionized water and calcium hydroxide, be heated to 80～85 ℃, under agitation condition, add subsequently the thick product of sulphormethoxine, then regulate pH to 9.5～10.5, it is all dissolved;
(b) in container, add gac, filter to get filtrate stir 0.5～2 hour under 80～85 ℃ of conditions after;
(c) under 75～80 ℃ of conditions, in described filtrate, drip glacial acetic acid solution, regulate pH to 5.1～5.4, staticly settle rear centrifuge dehydration and get filter residue; In step (c), it is cooling that described glacial acetic acid solution is placed in ice-water bath by filtrate after dripping.
Optimally, it also comprises that step (d) is placed in described filter residue at 100～120 ℃ and is dried 2～6 hours.
Optimally, in step (a), described calcium hydroxide at least divides three times and adds.
Optimally, the mass concentration of described glacial acetic acid solution is 25～20%.
Further, in step (d), after described filter residue and drying, be cooled to 45 ℃ with bottom discharge.
Because technique scheme is used, the present invention compared with prior art has following advantages: the purify method of sulphormethoxine of the present invention, cooling by filtrate being placed in to ice-water bath in the time that dropping glacial acetic acid solution staticly settles, can make sulphormethoxine precipitate rapidly, can get rid of the interference of other composition, improve purity and the productive rate of sulphormethoxine.
Embodiment
The purify method of sulphormethoxine of the present invention, comprises the following steps successively, (a) in reaction vessel, adds deionized water and calcium hydroxide, be heated to 80～85 ℃, under agitation condition, add subsequently the thick product of sulphormethoxine, then regulate pH to 9.5～10.5, it is all dissolved; (b) in container, add gac, filter to get filtrate stir 0.5～2 hour under 80～85 ℃ of conditions after; (c) under 75～80 ℃ of conditions, in described filtrate, drip glacial acetic acid solution, regulate pH to 5.1～5.4, staticly settle rear centrifuge dehydration and get filter residue; In step (c), it is cooling that described glacial acetic acid solution is placed in ice-water bath by filtrate after dripping.Cooling by filtrate being placed in to ice-water bath in the time that dropping glacial acetic acid solution staticly settles, can make sulphormethoxine precipitate rapidly, can get rid of the interference of other composition, improve purity and the productive rate of sulphormethoxine.
In order to get rid of the impact of moisture on sulphormethoxine, after step (c), also should comprise: step (d) is placed in described filter residue at 100～120 ℃ and is dried 2～6 hours, thoroughly removes moisture, should be cooled to subsequently 45 ℃ with bottom discharge.Because calcium hydroxide is slightly soluble in water, and in dissolution process, discharge a large amount of heats, it should at least divide and add for three times, and controls temperature and be no more than 80 degrees Celsius.The mass concentration of glacial acetic acid solution is preferably 25～20%, can not be too dense, otherwise be difficult to system pH to be controlled in 5.1～5.4.
Below in conjunction with specific embodiment, the present invention is described in more detail:
Embodiment 1
This example provides a kind of method of the sulphormethoxine of purifying, and concrete charge ratio is as shown in table 1:
Table 1 reaction raw materials and charge ratio thereof
| Material name | Charging capacity (kg) | Molecular weight | Remarks |
| The thick product of sulphormethoxine | Complete batch | 310.33 | ? |
| Deionized water | 2400 | 18 | ? |
| Calcium hydroxide | 20 | 74.08 | ? |
| Gac | 12.5 | 12 | ? |
| Glacial acetic acid | 35 | 60 | ? |
Specific operation process is as follows:
(a) in reaction vessel, add deionized water and calcium hydroxide, be heated to 80～85 ℃, under agitation condition, add subsequently the thick product of sulphormethoxine, then regulate pH to 9.5～10.5, the thick product of sulphormethoxine is all dissolved;
(b) in container, add gac, under 80～85 ℃ of conditions, stir after 1 hour, have the monolithic Filter Press of two metafiltration cloth one deck filter paper to obtain filtrate by pin it;
(c) under 75～80 ℃ of conditions to the glacial acetic acid solution that drips 25～30wt% in described filtrate, regulate pH to 5.1～5.4, be placed in ice-water bath cooling, staticly settle 5～15 minutes after centrifuge dehydration get filter residue;
(d) described filter residue is placed at 100～120 ℃ and is dried 4 hours, be cooled to 45 ℃ with bottom discharge.
Above-described embodiment is only explanation technical conceive of the present invention and feature; its object is to allow person skilled in the art can understand content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences that spirit is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (5)
1. the purify method of sulphormethoxine, comprises the following steps successively,
(a) in reaction vessel, add deionized water and calcium hydroxide, be heated to 80～85 ℃, under agitation condition, add subsequently the thick product of sulphormethoxine, then regulate pH to 9.5～10.5, it is all dissolved;
(b) in container, add gac, filter to get filtrate stir 0.5～2 hour under 80～85 ℃ of conditions after;
(c) under 75～80 ℃ of conditions, in described filtrate, drip glacial acetic acid solution, regulate pH to 5.1～5.4, staticly settle rear centrifuge dehydration and get filter residue;
It is characterized in that: in step (c), it is cooling that described glacial acetic acid solution is placed in ice-water bath by filtrate after dripping.
2. the method for purification sulphormethoxine according to claim 1, is characterized in that: it also comprises that step (d) is placed in described filter residue at 100～120 ℃ and is dried 2～6 hours.
3. the method for purification sulphormethoxine according to claim 1, is characterized in that: in step (a), described calcium hydroxide at least divides three times and adds.
4. the method for purification sulphormethoxine according to claim 1, is characterized in that: the mass concentration of described glacial acetic acid solution is 25～20%.
5. the method for purification sulphormethoxine according to claim 2, is characterized in that: in step (d), be cooled to 45 ℃ with bottom discharge after described filter residue and drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410083160.7A CN103910685A (en) | 2014-03-10 | 2014-03-10 | Method used for purifying sulfadimoxine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410083160.7A CN103910685A (en) | 2014-03-10 | 2014-03-10 | Method used for purifying sulfadimoxine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103910685A true CN103910685A (en) | 2014-07-09 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410083160.7A Pending CN103910685A (en) | 2014-03-10 | 2014-03-10 | Method used for purifying sulfadimoxine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103910685A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557736A (en) * | 2014-12-13 | 2015-04-29 | 常熟市金申医化制品有限责任公司 | Purification method of sulfadoxine |
| CN104557735A (en) * | 2014-12-04 | 2015-04-29 | 重庆康乐制药有限公司 | Preparation method of high-purity sulfadoxine |
| CN112592319A (en) * | 2020-12-22 | 2021-04-02 | 重庆康乐制药有限公司 | Refining method of high-quality sulfadoxine |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RO63267A2 (en) * | 1974-01-09 | 1978-02-20 | Medicamente Intreprinderea De | PROCESS FOR OBTAINING 4,6-DIHYDROXY-5-METHOXYPYRIMIDINE |
| CN1569843A (en) * | 2004-04-29 | 2005-01-26 | 常熟市南湖实业化工厂 | Preparation method for sulfadoxine |
| CN102304095A (en) * | 2011-09-23 | 2012-01-04 | 常熟市南湖实业化工有限公司 | Preparation method of sulfadoxine |
| CN102391190A (en) * | 2011-09-30 | 2012-03-28 | 常熟市金申医化制品有限责任公司 | Method for preparing sulfadoxine |
-
2014
- 2014-03-10 CN CN201410083160.7A patent/CN103910685A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RO63267A2 (en) * | 1974-01-09 | 1978-02-20 | Medicamente Intreprinderea De | PROCESS FOR OBTAINING 4,6-DIHYDROXY-5-METHOXYPYRIMIDINE |
| CN1569843A (en) * | 2004-04-29 | 2005-01-26 | 常熟市南湖实业化工厂 | Preparation method for sulfadoxine |
| CN102304095A (en) * | 2011-09-23 | 2012-01-04 | 常熟市南湖实业化工有限公司 | Preparation method of sulfadoxine |
| CN102391190A (en) * | 2011-09-30 | 2012-03-28 | 常熟市金申医化制品有限责任公司 | Method for preparing sulfadoxine |
Non-Patent Citations (1)
| Title |
|---|
| 上海第二制药厂: "4-磺胺-5 , 6-二甲氧基嘧啶(周效磺胺) 的合成", 《医药工业》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557735A (en) * | 2014-12-04 | 2015-04-29 | 重庆康乐制药有限公司 | Preparation method of high-purity sulfadoxine |
| CN104557735B (en) * | 2014-12-04 | 2017-03-22 | 重庆康乐制药有限公司 | Preparation method of sulfadoxine |
| CN104557736A (en) * | 2014-12-13 | 2015-04-29 | 常熟市金申医化制品有限责任公司 | Purification method of sulfadoxine |
| CN112592319A (en) * | 2020-12-22 | 2021-04-02 | 重庆康乐制药有限公司 | Refining method of high-quality sulfadoxine |
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Application publication date: 20140709 |