CN105418474A - Refining method for main ring of aztreonam - Google Patents
Refining method for main ring of aztreonam Download PDFInfo
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- CN105418474A CN105418474A CN201510969451.0A CN201510969451A CN105418474A CN 105418474 A CN105418474 A CN 105418474A CN 201510969451 A CN201510969451 A CN 201510969451A CN 105418474 A CN105418474 A CN 105418474A
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- Prior art keywords
- main ring
- aztreonam
- purification
- aztreonam main
- ring according
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D205/00—Heterocyclic compounds containing four-membered rings with one nitrogen atom as the only ring hetero atom
- C07D205/02—Heterocyclic compounds containing four-membered rings with one nitrogen atom as the only ring hetero atom not condensed with other rings
- C07D205/06—Heterocyclic compounds containing four-membered rings with one nitrogen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D205/08—Heterocyclic compounds containing four-membered rings with one nitrogen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with one oxygen atom directly attached in position 2, e.g. beta-lactams
- C07D205/085—Heterocyclic compounds containing four-membered rings with one nitrogen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with one oxygen atom directly attached in position 2, e.g. beta-lactams with a nitrogen atom directly attached in position 3
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of medicine synthesis, and particularly relates to a refining method for a main ring of aztreonam. The method comprises the steps of: adding a coarse product of the main ring of aztreonam into a reaction kettle; adding a mixed solution and raising the temperature for dissolution; after dissolution, reducing the temperature to carry out crystallization; dumping materials to obtain a wet product; and drying the wet product to obtain white-like crystal powder, wherein mother liquor can be recycled and applied circularly. The refining method provided by the invention is simple to operate, relatively high in yield and low in cost, and high-purity main ring of aztreonam can be obtained.
Description
Technical field
The invention belongs to medical synthesis technical field, be specifically related to a kind of process for purification of aztreonam main ring.
Background technology
Aztreonam is monocycle beta-lactam class microbiotic, has good therapeutic action to gram positive bacterial infection.Aztreonam main ring is the important intermediate of synthesis aztreonam, and its quality and purity directly affect the quality of ceftazime active ester, and then affect quality and the production cost of ceftazime medicine.Purity due to aztreonam main ring is lower is the cost of restriction aztreonam bulk drug and the important factor of quality.The current report to the process for purification of aztreonam main ring and document do not have.
Summary of the invention
The object of this invention is to provide a kind of process for purification of aztreonam main ring, simply, yield is high, cost is low, be easy to control.
The process for purification of aztreonam main ring of the present invention is in reactor, add aztreonam main ring crude product, adds mixing solutions rising temperature for dissolving, molten clear after lower the temperature crystallization, get rid of material, wet product drying obtains off-white color crystalline powder, and Recycling Mother Solution is applied mechanically.
Described mixed solvent is the mixture of water and organic solvent.
Described organic solvent is the one in DMF, methyl alcohol, ethanol, Virahol or the trimethyl carbinol, preferred alcohol.
Described water and the volume ratio of organic solvent are 10-14:1.
The volume of described mixing solutions is 11-15 times of aztreonam main ring crude product quality, and volume is in L, and quality is in kg.
Described rising temperature for dissolving temperature is 55-75 DEG C.
The temperature of described cooling crystallization is 0-10 DEG C.
Described recycled number of times is 4-6 time.
The present invention compared with prior art, has following beneficial effect:
The present invention is simple to operate, and yield is higher, and cost is low and can obtain the bent southern main ring of high purity ammonia.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
In 500L reactor, add aztreonam main ring crude product 20kg, then add 240L water and 20L ethanol, be warming up to 65 DEG C and stir 20min dissolving, molten clear after be then cooled to 5 DEG C and get rid of material, wet product drying obtains 19.83kg aztreonam main ring, and purity is 99.87%, and mother liquor applies mechanically 5 times continuously.
Embodiment 2
In 500L reactor, add aztreonam main ring crude product 20kg, then add 200L water and 20L ethanol, be warming up to 55 DEG C and stir 20min dissolving, molten clear after be then cooled to 2 DEG C and get rid of material, wet product drying obtains 19.65kg aztreonam main ring, and purity is 99.95%, and mother liquor applies mechanically 4 times continuously.
Embodiment 3
In 500L reactor, add aztreonam main ring crude product 20kg, then add 280L water and 20L ethanol, be warming up to 75 DEG C and stir 15min dissolving, molten clear after be then cooled to 10 DEG C and get rid of material, wet product drying obtains 19.91kg aztreonam main ring, and purity is 99.92%, and mother liquor applies mechanically 6 times continuously.
Embodiment 4
In 500L reactor, add aztreonam main ring crude product 20kg, then add 240L water and 20L ethanol, be warming up to 61 DEG C and stir 20min dissolving, molten clear after be then cooled to 5 DEG C and get rid of material, wet product drying obtains 19.70kg aztreonam main ring, and purity is 99.92%, and mother liquor applies mechanically 5 times continuously.
Embodiment 5
In 500L reactor, add aztreonam main ring crude product 20kg, then add 220L water and 20L ethanol, be warming up to 73 DEG C and stir 25min dissolving, molten clear after be then cooled to 4 DEG C and get rid of material, wet product drying obtains 19.73kg aztreonam main ring, and purity is 99.89%, and mother liquor applies mechanically 6 times continuously.
Embodiment 6
In 500L reactor, add aztreonam main ring crude product 20kg, then add 2600L water and 20L ethanol, be warming up to 67 DEG C and stir 20min dissolving, molten clear after be then cooled to 7 DEG C and get rid of material, wet product drying obtains 19.94kg aztreonam main ring, and purity is 99.96%, and mother liquor applies mechanically 4 times continuously.
Embodiment 7
In 500L reactor, add aztreonam main ring crude product 20kg, then add 240L water and 20L methyl alcohol, be warming up to 64 DEG C and stir 20min dissolving, molten clear after be then cooled to 5 DEG C and get rid of material, wet product drying obtains 19.90kg aztreonam main ring, and purity is 99.98%, mother liquid recycle 5 times.
Claims (8)
1. a process for purification for aztreonam main ring, is characterized in that in reactor, add aztreonam main ring crude product, adds mixing solutions rising temperature for dissolving, molten clear after lower the temperature crystallization, get rid of material, wet product drying obtains off-white color crystalline powder, and Recycling Mother Solution is applied mechanically.
2. the process for purification of aztreonam main ring according to claim 1, is characterized in that described mixed solvent is the mixture of water and organic solvent.
3. the process for purification of aztreonam main ring according to claim 2, is characterized in that described organic solvent is the one in DMF, methyl alcohol, ethanol, Virahol or the trimethyl carbinol.
4. the process for purification of aztreonam main ring according to claim 2, is characterized in that the volume ratio of described water and organic solvent is 10-14:1.
5. the process for purification of aztreonam main ring according to claim 1, it is characterized in that the volume of described mixing solutions is 11-15 times of aztreonam main ring crude product quality, volume is in L, and quality is in kg.
6. the process for purification of aztreonam main ring according to claim 1, is characterized in that described rising temperature for dissolving temperature is 55-75 DEG C.
7. the process for purification of aztreonam main ring according to claim 1, is characterized in that the temperature of described cooling crystallization is 0-10 DEG C.
8. the process for purification of aztreonam main ring according to claim 1, is characterized in that described recycled number of times is 4-6 time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510969451.0A CN105418474A (en) | 2015-12-21 | 2015-12-21 | Refining method for main ring of aztreonam |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510969451.0A CN105418474A (en) | 2015-12-21 | 2015-12-21 | Refining method for main ring of aztreonam |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105418474A true CN105418474A (en) | 2016-03-23 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510969451.0A Pending CN105418474A (en) | 2015-12-21 | 2015-12-21 | Refining method for main ring of aztreonam |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102285907A (en) * | 2011-09-20 | 2011-12-21 | 四川武胜春瑞医药化工有限公司 | Method for preparing aztreonam monocyclic parent nucleus |
| CN102584811A (en) * | 2011-12-29 | 2012-07-18 | 蚌埠丰原涂山制药有限公司 | Method for preparing aztreonam |
| CN104592081A (en) * | 2015-02-06 | 2015-05-06 | 石家庄万业化工科技有限公司 | Synthesis method of aztreonam main ring |
-
2015
- 2015-12-21 CN CN201510969451.0A patent/CN105418474A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102285907A (en) * | 2011-09-20 | 2011-12-21 | 四川武胜春瑞医药化工有限公司 | Method for preparing aztreonam monocyclic parent nucleus |
| CN102584811A (en) * | 2011-12-29 | 2012-07-18 | 蚌埠丰原涂山制药有限公司 | Method for preparing aztreonam |
| CN104592081A (en) * | 2015-02-06 | 2015-05-06 | 石家庄万业化工科技有限公司 | Synthesis method of aztreonam main ring |
Non-Patent Citations (2)
| Title |
|---|
| 史刚: "氨曲南主环合成工艺研究", 《中国优秀硕士学位论文全文数据库》 * |
| 李丽娟: "《药物合成技术》", 31 December 2010 * |
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Application publication date: 20160323 |