CN101307062B - Straight method for producing 7-amino-3-descetoxy-cephalosporanic acid - Google Patents
Straight method for producing 7-amino-3-descetoxy-cephalosporanic acid Download PDFInfo
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- CN101307062B CN101307062B CN 200810100621 CN200810100621A CN101307062B CN 101307062 B CN101307062 B CN 101307062B CN 200810100621 CN200810100621 CN 200810100621 CN 200810100621 A CN200810100621 A CN 200810100621A CN 101307062 B CN101307062 B CN 101307062B
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Abstract
The invention discloses a straight-through method for producing 7-amino-3-desacetoxy-cephalosporanic acid, comprising oxidation and ring enlargement. The invention is characterized by pressing a ring enlarging solution in the ring enlargement process into a hydrolyzing kettle when the ring enlarging solution is still hot; adding water which is equal to 80 percent of the total volume of the ring enlarging solution, simultaneously adjusting the pH value of the solution by 20 percent ammonia to 8.5, and keeping the adjusted solution stand after the adjusted solution is stirred and hydrolyzed to separate an aqueous phase; adding water which is equal to 40 percent of the total volume of the ring enlarging solution once again into the solution, keeping the solution stand after the solution is mixed and hydrolyzed to separate an aqueous phase, and sending an ortho-toluene organic phase in a ring enlargement system to a treatment position; adding an extracting agent into the aqueous phases which are separated twice according to a volume ratio of 1 to 0.8, and stirring and keeping the solution stand to separate an aqueous phase; adding the extracting agent which is equal to 30 percent of the volume of the aqueous phase into the aqueous phase twice, stirring and keeping the solution stand to separate an aqueous phase; stirring and decoloring the aqueous phase which is added with active carbon which is equal to 1 percent the aqueous phase by weight; and pressing the solution into a cracking kettle through a filter for cracking. The method has the advantages of simple process, small wasterwater discharge and so on.
Description
Technical field:
The present invention relates to the method for a kind of 7-of production amino-3-desacetoxycephalosporanic acid.
Background technology:
7-ADCA (7-amino-3-desacetoxycephalosporanic acid) is mainly used in the synthetic of oral class cynnematins such as Cephalexin Monohydrate Micro/Compacted, S 578, Cephradine, Cefaclor, cefetamet.
7-ADCA production mainly comprises oxidation section, ring expansion workshop section, three big steps of cracking workshop section; Traditional technology is with three step independent operations, and each step is all taken out the use that intermediates are used for next workshop section.Complex process, discharge of wastewater is many, and efficiency is low.
Summary of the invention:
The object of the present invention is to provide a kind of technology simple, the method through of production 7-amino-3-desacetoxycephalosporanic acid that discharge of wastewater is few.
Technical solution of the present invention is:
A kind of method through of producing 7-amino-3-desacetoxycephalosporanic acid, comprise oxidation, ring expansion, it is characterized in that: the ring expansion liquid in the ring expansion process is pressed into hydrolysis kettle while hot, add the water that is equivalent to ring expansion liquid cumulative volume 80%, transfer PH=8.5 with 20% ammoniacal liquor simultaneously, leave standstill after stirring hydrolysis, tell water, add the water that is equivalent to ring expansion liquid cumulative volume 40% once more, leave standstill after stirring hydrolysis, tell water, the former toluene organic phase in the ring expansion system is sent and is handled the post, the aqueous phase of telling at secondary adds extraction agent by 1: 0.8 volume, stir, leave standstill, tell water, add the extraction agent that is equivalent to water volume 30%, stir at the aqueous phase secondary, leave standstill, tell water, the gac that water adds water weight 1% stirs, decolour, be pressed onto by strainer and carry out cracking in the cracking still.
Extraction agent is handled the back recycled; The extraction agent treatment process is: extraction agent is adopted first air distillation, and vacuum distilling again, extraction component wherein, remainder is delivered to boiler and is burned with the method extraction of decompression, remaining raffinate, and the steam of generation uses for producing.
Extraction agent is a kind of or blending ingredients in methylene dichloride, trichloromethane, benzene, DMF, the isopropylcarbinol.
Advantage of the present invention: (1) has reduced technological process, need not to take out the acid of intermediates ring expansion, and 14 original operations are reduced to 10 workshop sections, has reduced pilot process, and the yield that makes whole technology is by 40% original raising 44%.(2) improved quality product, improved the quality of ring expansion acid by improvement, the content that makes the finished product is brought up to more than 98.5% by original 97%.Acid consumption when (3) having reduced the acid out product, the consumption of ammonia when dissolving ammoniacal liquor, cost decreases per ton nearly 1%, (4) have lacked the step of acid out, have reduced labour intensity, have improved efficient.(5) reduce the discharging of the waste water of taking out ring expansion when acid, reduced the discharging of waste water, saved three wastes processing cost, protected on-the-spot operating environment and social environment.
The invention will be further described below in conjunction with embodiment:
A kind of method through of producing 7-amino-3-desacetoxycephalosporanic acid comprises oxidation, ring expansion, and ring expansion liquid is pressed into hydrolysis kettle while hot, add the water of ring expansion liquid cumulative volume 80%, transfer PH=8.5 with 20% ammoniacal liquor simultaneously, stir hydrolysis 20 minutes, left standstill 10 minutes, and told water.The water that adds ring expansion liquid cumulative volume 40% once more stirs hydrolysis 20 minutes, leaves standstill 30 minutes, tells water, and the former toluene organic phase in the ring expansion system is sent and handled the post.Add extraction agent methylene dichloride (or a kind of or blending ingredients in the trichloromethane, benzene, DMF, isopropylcarbinol) by 1: 0.8 volume at aqueous phase that secondary is told, stir 20 minutes, leave standstill 10 minutes, tell water.Add the extraction agent of 30% volume at the aqueous phase secondary, stir 20 minutes, leave standstill 30 minutes, tell water.The gac that water adds weight 1% stirs, and decolouring is 30 minutes under the vacuum under the 10mmHg pressure, is pressed onto by strainer and carries out cracking in the cracking still.Extraction agent removes to handle the back recycled.Processing scheme: extraction agent is adopted first air distillation, vacuum distilling again, extraction component wherein, the method extraction of residue decompression.Remaining raffinate is delivered to boiler and is burned, and the steam of generation uses for producing.
Claims (2)
1. method through of producing 7-amino-3-desacetoxycephalosporanic acid, comprise oxidation, ring expansion, it is characterized in that: the ring expansion liquid in the ring expansion process is pressed into hydrolysis kettle while hot, add the water that is equivalent to ring expansion liquid cumulative volume 80%, transfer pH=8.5 with 20% ammoniacal liquor simultaneously, leave standstill after stirring hydrolysis, tell water, add the water that is equivalent to ring expansion liquid cumulative volume 40% once more, leave standstill after stirring hydrolysis, tell water, the former toluene organic phase in the ring expansion system is sent and is handled the post, the aqueous phase of telling at secondary adds extraction agent by 1: 0.8 volume, stir, leave standstill, tell water, add the extraction agent that is equivalent to water volume 30%, stir at the aqueous phase secondary, leave standstill, tell water, the gac that water adds water weight 1% stirs, decolour, be pressed onto by strainer and carry out cracking in the cracking still.
2. the method through of production 7-amino according to claim 1-3-desacetoxycephalosporanic acid, it is characterized in that: extraction agent is a kind of or blending ingredients in methylene dichloride, trichloromethane, benzene, DMF, the isopropylcarbinol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810100621 CN101307062B (en) | 2008-05-12 | 2008-05-12 | Straight method for producing 7-amino-3-descetoxy-cephalosporanic acid |
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| CN 200810100621 CN101307062B (en) | 2008-05-12 | 2008-05-12 | Straight method for producing 7-amino-3-descetoxy-cephalosporanic acid |
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| CN101307062A CN101307062A (en) | 2008-11-19 |
| CN101307062B true CN101307062B (en) | 2011-04-13 |
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| CN 200810100621 Active CN101307062B (en) | 2008-05-12 | 2008-05-12 | Straight method for producing 7-amino-3-descetoxy-cephalosporanic acid |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102659195B (en) * | 2012-05-14 | 2013-05-15 | 江苏九九久科技股份有限公司 | Processing method for chemical production wastewater |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5302713A (en) * | 1992-03-31 | 1994-04-12 | Industrial Technology Research Institute | Method for the preparation of Δ3 -7-substituted amino desacetoxy cephalosporanic acid |
| CN1201795A (en) * | 1998-05-22 | 1998-12-16 | 范伟光 | Preparation of 7-amino-deacetylated cefa-alkylation acid |
| CN1840687A (en) * | 2006-01-25 | 2006-10-04 | 周新基 | Method for fermentation preparation of 7-amino-3-deacetoxy cephalosporanic acid |
-
2008
- 2008-05-12 CN CN 200810100621 patent/CN101307062B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5302713A (en) * | 1992-03-31 | 1994-04-12 | Industrial Technology Research Institute | Method for the preparation of Δ3 -7-substituted amino desacetoxy cephalosporanic acid |
| CN1201795A (en) * | 1998-05-22 | 1998-12-16 | 范伟光 | Preparation of 7-amino-deacetylated cefa-alkylation acid |
| CN1840687A (en) * | 2006-01-25 | 2006-10-04 | 周新基 | Method for fermentation preparation of 7-amino-3-deacetoxy cephalosporanic acid |
Non-Patent Citations (4)
| Title |
|---|
| 李永刚 等.从青霉素G 生产7-氨基脱乙酰氧基头孢烷酸.中国医药工业杂志31 8.2000,31(8),376-380. |
| 李永刚等.从青霉素G 生产7-氨基脱乙酰氧基头孢烷酸.中国医药工业杂志31 8.2000,31(8),376-380. * |
| 李葵英 等.7 - 氨基去乙酰氧基头孢烷酸合成工艺改进.广东药学院学报19 3.2003,19(3),247-248. |
| 李葵英等.7-氨基去乙酰氧基头孢烷酸合成工艺改进.广东药学院学报19 3.2003,19(3),247-248. * |
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Address after: 226407 Rudong Economic Development Zone, Nantong, the Yellow Sea, No., No. three road, No. 12 Patentee after: Jiangsu BICON Pharmaceutical Co., Ltd. Address before: 226401 Jiangsu Matang Town County of Rudong province Jianshe Road No. 40 Patentee before: Jiangsu Jiujiujiu Technology Co., Ltd. |
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Effective date of registration: 20171227 Address after: 226407 Rudong Economic Development Zone, Nantong, the Yellow Sea, No., No. three road, No. 12 Patentee after: Jiangsu nine Jiangsu jiujiujiu Technology Co. Ltd. Address before: 226407 Rudong Economic Development Zone, Nantong, the Yellow Sea, No., No. three road, No. 12 Patentee before: Jiangsu BICON Pharmaceutical Co., Ltd. |
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Effective date of registration: 20200618 Address after: 312300 No.3, Weiwu Road, Shangyu economic and Technological Development Zone, Shangyu District, Shaoxing City, Zhejiang Province Patentee after: ZHEJIANG ZHEBANG PHARMACEUTICAL Co.,Ltd. Address before: 226407 No. three, 12 the Yellow Sea Road, Rudong Coastal Economic Development Zone, Nantong, Jiangsu, China Patentee before: JIANGSU JIUJIUJIU TECHNOLOGY Co.,Ltd. |