CN104130186A - Method for improving salicylazosulfapyridine refining production efficiency - Google Patents
Method for improving salicylazosulfapyridine refining production efficiency Download PDFInfo
- Publication number
- CN104130186A CN104130186A CN201410307614.4A CN201410307614A CN104130186A CN 104130186 A CN104130186 A CN 104130186A CN 201410307614 A CN201410307614 A CN 201410307614A CN 104130186 A CN104130186 A CN 104130186A
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- CN
- China
- Prior art keywords
- refining
- salicylazosulfapyridine
- solid
- production efficiency
- sulfasalazine
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- 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
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/72—Nitrogen atoms
- C07D213/76—Nitrogen atoms to which a second hetero atom is attached
Abstract
A disclosed method for improving salicylazosulfapyridine refining production efficiency comprises: cooling a salicylazosulfapyridine suspension in a crystallization pan to 5-10 DEG C, putting in a dissolving filter to filter, pressing the material with nitrogen to dry, keeping the press-dried material in the dissolving filter, directly adding an aqueous solution of glacial acetic acid for next-step refining into the dissolving filter, stirring the solid material to be at a suspended state, and directly pressing the solid-liquid mixture into a next-step refining reaction pan, so as to finish the whole material discharging, transferring and feeding work. According to the method, the technology operation time is shortened, and all operations are performed in a sealed system. The work labor intensity is substantially reduced and operation accords with GMP requirements. Also, environmental pollution is reduced and the risk that the material is polluted because of long-term exposure is avoided.
Description
Technical field
The invention belongs to field of medicine and chemical technology, be specifically related to a kind of method that improves the refining production efficiency of sulfasalazine.
Background technology
5-[p-(2-pyridine sulfamic) benzene] Olsalazine; general sulfasalazine by name; be for No. CAS 599-79-1; nineteen fifty goes on the market in the U.S.; 1999 in Discussion on Chinese Listed, be very old product, but the market requirement is still very large; main formulation is Tablet and Capsula, is used for the treatment of inflammatory bowel and ulcerative colitis.Sulfasalazine is disulfonamide, is mainly used in treating ulcerative colitis (UC), and its formulation is divided into two kinds of tablet and suppositorys.
In sulfasalazine production process, exist a large amount of solid-liquid feed separation, during general manufacturer production, all adopt whizzer separating and filtering, material being taken out in whizzer again, dropped into again reactor, labor strength is very large, and the long-time exposure of material easily causes material to pollute, and does not reach GMP (Good Manufacturing Practice) production requirement, particularly production operation and very easily causes the pollution of environment.Present method is used a kind of novel equipment dissolution filter device, solid-liquid two phase materials are after dissolution filter device filters, solid materials is not taken out, directly next step refining glacial acetic acid aqueous solution used is added to dissolution filter device, solid materials is broken into outstanding mixed shape, by nitrogen, be depressed into next step refining reaction pot again, the process that the use of this kind of equipment has been got rid of the discharging of whizzer solid and fed intake to refining reaction pot, workman's labour intensity reduces greatly, owing to having reduced workman, contact with material simultaneously, reduce widely material and contacted the Occupational Disease Hazards causing with workman.
Summary of the invention
The object of this part is to summarize some aspects of embodiments of the invention and briefly introduces some preferred embodiments.In this part and the application's specification digest and denomination of invention, may do a little simplification or omit to avoid the making object of this part, specification digest and denomination of invention fuzzy, and this simplification or omit can not be for limiting the scope of the invention.
Problem in view of existing in above-mentioned and/or existing sulfasalazine Refining process, has proposed the present invention.
Therefore, the object of this invention is to provide a kind of method that improves the refining production efficiency of sulfasalazine, a kind of solid-liquid feed separation method in sulfasalazine production process is provided.
For solving the problems of the technologies described above, the invention provides following technical scheme: a kind of method that improves the refining production efficiency of sulfasalazine, comprise, the outstanding mixed liquid of the sulfasalazine that is cooled to 5～10 ℃ in crystallizing pan is put into dissolution filter device, by nitrogen, material is pressed dry, after pressing dry, material is not taken out, directly by the glacial acetic acid aqueous solution of next step refining use, be added in described dissolution filter device, solid materials is broken into after outstanding mixed shape, directly solid-liquid mixture is pressed into next step refining reaction pot, completes whole discharging, the work of shifting, feed intake.
Remarkable advantage of the present invention:
1, operation is all carried out in airtight system; Operation meets GMP requirement;
2, labor intensity reduces greatly, reduces operative employee and contacts with material, has reduced Occupational Disease Hazards risk.
3, reducing material environmental pollution has also avoided long-time exposure of material to bring contaminated risk.
4, the process time shortens, every batch of productive manpower discharging of former technique, clear out a gathering place, the approximately 5 hours overall process that feeds intake again time, use instead after dissolution filter device, only increase the reinforced and outstanding mixed liquid of a step liquid and turn material, overall process time 2 h; After new installation is used, than former technique, shorten 3 hours, working efficiency improves greatly.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with specific embodiment, the specific embodiment of the present invention is described in detail.
A lot of details have been set forth in the following description so that fully understand the present invention, but the present invention can also adopt other to be different from alternate manner described here and implement, those skilled in the art can do similar popularization without prejudice to intension of the present invention in the situation that, so the present invention is not subject to the restriction of following public specific embodiment.
Secondly, alleged " embodiment " or " embodiment " refers to special characteristic, structure or the characteristic that can be contained at least one implementation of the present invention herein.Different local in this manual " in one embodiment " that occur not all refer to same embodiment, neither be independent or the embodiment mutually exclusive with other embodiment optionally.
Embodiment 1:
The outstanding mixed liquid of the sulfasalazine that is cooled to 5 ℃ in crystallizing pan is put into dissolution filter device to be filtered, by nitrogen, material is pressed dry, after pressing dry, material is not taken out, directly by the glacial acetic acid aqueous solution of next step refining use, 50 minutes time, be added in described dissolution filter device, solid materials is broken into after outstanding mixed shape, directly solid-liquid mixture is pressed into next step refining reaction pot, turn 1 hour material time, complete whole discharging, the work 1 hour 50 minutes of shifting, feed intake, transhipment material 1.2T.
Embodiment 2:
The outstanding mixed liquid of the sulfasalazine that is cooled to 7 ℃ in crystallizing pan is put into dissolution filter device to be filtered, by nitrogen, material is pressed dry, after pressing dry, material is not taken out, directly by the glacial acetic acid aqueous solution of next step refining use, 60 minutes time, be added in described dissolution filter device, solid materials is broken into after outstanding mixed shape, directly solid-liquid mixture is pressed into next step refining reaction pot, turn 1 hour material time, complete whole discharging, the work 2 hours of shifting, feed intake, transhipment material 1.3T.
Case 3:
The outstanding mixed liquid of the sulfasalazine that is cooled to 10 ℃ in crystallizing pan is put into dissolution filter device to be filtered, by nitrogen, material is pressed dry, after pressing dry, material is not taken out, directly by the glacial acetic acid aqueous solution of next step refining use, 55 minutes time, be added in described dissolution filter device, solid materials is broken into after outstanding mixed shape, directly solid-liquid mixture is pressed into next step refining reaction pot, turn 1 hour 20 minutes material time, complete whole discharging, the work 2 hours 15 minutes of shifting, feed intake, transhipment material 1.3T.
It should be noted that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (1)
1. a method that improves the refining production efficiency of sulfasalazine, is characterized in that: comprises,
The outstanding mixed liquid of the sulfasalazine that is cooled to 5～10 ℃ in crystallizing pan is put into dissolution filter device to be filtered, by nitrogen, material is pressed dry, after pressing dry, material is not taken out, directly by the glacial acetic acid aqueous solution of next step refining use, be added in described dissolution filter device, solid materials is broken into after outstanding mixed shape, directly solid-liquid mixture is pressed into next step refining reaction pot, complete whole discharging, the work of shifting, feed intake.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410307614.4A CN104130186A (en) | 2014-06-30 | 2014-06-30 | Method for improving salicylazosulfapyridine refining production efficiency |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410307614.4A CN104130186A (en) | 2014-06-30 | 2014-06-30 | Method for improving salicylazosulfapyridine refining production efficiency |
Publications (1)
| Publication Number | Publication Date |
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| CN104130186A true CN104130186A (en) | 2014-11-05 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410307614.4A Pending CN104130186A (en) | 2014-06-30 | 2014-06-30 | Method for improving salicylazosulfapyridine refining production efficiency |
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| CN (1) | CN104130186A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105085566A (en) * | 2015-09-01 | 2015-11-25 | 江苏瑞克医药科技有限公司 | Method and equipment for producing imipenem intermediate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1296655A (en) * | 1970-03-06 | 1972-11-15 | ||
| GB2041958A (en) * | 1979-01-29 | 1980-09-17 | Johansson J A O | Medical preparations containing salicylazosulfa pyridine |
| CN1566097A (en) * | 2003-07-01 | 2005-01-19 | 上海三维制药有限公司 | Purification process for 5-[pair-(2-pyridine sulfamic) benzene] azo salicylic acid |
| CN103044323A (en) * | 2012-12-27 | 2013-04-17 | 浙江九洲药业股份有限公司 | Method for purifying salazosulfapyridine |
-
2014
- 2014-06-30 CN CN201410307614.4A patent/CN104130186A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1296655A (en) * | 1970-03-06 | 1972-11-15 | ||
| GB2041958A (en) * | 1979-01-29 | 1980-09-17 | Johansson J A O | Medical preparations containing salicylazosulfa pyridine |
| CN1566097A (en) * | 2003-07-01 | 2005-01-19 | 上海三维制药有限公司 | Purification process for 5-[pair-(2-pyridine sulfamic) benzene] azo salicylic acid |
| CN103044323A (en) * | 2012-12-27 | 2013-04-17 | 浙江九洲药业股份有限公司 | Method for purifying salazosulfapyridine |
Non-Patent Citations (2)
| Title |
|---|
| 汪良明，等: "溶解过滤器代替离心机的应用", 《浙江化工》 * |
| 金灿，等: "柳氮磺胺吡啶的合成工艺改进", 《合成化学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105085566A (en) * | 2015-09-01 | 2015-11-25 | 江苏瑞克医药科技有限公司 | Method and equipment for producing imipenem intermediate |
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| C12 | Rejection of a patent application after its publication | ||
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Application publication date: 20141105 |