CN111072497B - Method for recovering N, N' -dibenzylethylenediamine salt from ion exchange resin to be regenerated of cefonicid sodium - Google Patents
Method for recovering N, N' -dibenzylethylenediamine salt from ion exchange resin to be regenerated of cefonicid sodium Download PDFInfo
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- CN111072497B CN111072497B CN201911073832.5A CN201911073832A CN111072497B CN 111072497 B CN111072497 B CN 111072497B CN 201911073832 A CN201911073832 A CN 201911073832A CN 111072497 B CN111072497 B CN 111072497B
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000003456 ion exchange resin Substances 0.000 title claims abstract description 28
- 229920003303 ion-exchange polymer Polymers 0.000 title claims abstract description 28
- NAXFZVGOZUWLEP-RFXDPDBWSA-L cefonicid sodium Chemical compound [Na+].[Na+].S([C@@H]1[C@@H](C(N1C=1C([O-])=O)=O)NC(=O)[C@H](O)C=2C=CC=CC=2)CC=1CSC1=NN=NN1CS([O-])(=O)=O NAXFZVGOZUWLEP-RFXDPDBWSA-L 0.000 title claims abstract description 24
- 229960004489 cefonicid Drugs 0.000 title claims abstract description 23
- JUHORIMYRDESRB-UHFFFAOYSA-N benzathine Chemical class C=1C=CC=CC=1CNCCNCC1=CC=CC=C1 JUHORIMYRDESRB-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 22
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000013078 crystal Substances 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000012065 filter cake Substances 0.000 claims abstract description 14
- 239000012670 alkaline solution Substances 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- 238000011084 recovery Methods 0.000 claims abstract description 11
- 239000011780 sodium chloride Substances 0.000 claims abstract description 11
- 239000002274 desiccant Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012445 acidic reagent Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 9
- 230000008025 crystallization Effects 0.000 claims abstract description 9
- 238000005191 phase separation Methods 0.000 claims abstract description 9
- 239000012074 organic phase Substances 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 238000000605 extraction Methods 0.000 claims abstract description 4
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical group CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical group [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 10
- 239000012452 mother liquor Substances 0.000 abstract description 4
- 229940079593 drug Drugs 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 239000013065 commercial product Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- GRONZTPUWOOUFQ-UHFFFAOYSA-M sodium;methanol;hydroxide Chemical compound [OH-].[Na+].OC GRONZTPUWOOUFQ-UHFFFAOYSA-M 0.000 description 2
- 206010005940 Bone and joint infections Diseases 0.000 description 1
- 229930186147 Cephalosporin Natural products 0.000 description 1
- 108090000204 Dipeptidase 1 Proteins 0.000 description 1
- 206010024971 Lower respiratory tract infections Diseases 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 206010040047 Sepsis Diseases 0.000 description 1
- 206010062255 Soft tissue infection Diseases 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 102000006635 beta-lactamase Human genes 0.000 description 1
- 229940124587 cephalosporin Drugs 0.000 description 1
- 150000001780 cephalosporins Chemical class 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000004260 plant-type cell wall biogenesis Effects 0.000 description 1
- CASUWPDYGGAUQV-UHFFFAOYSA-M potassium;methanol;hydroxide Chemical compound [OH-].[K+].OC CASUWPDYGGAUQV-UHFFFAOYSA-M 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 208000013223 septicemia Diseases 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000072 sodium resin Substances 0.000 description 1
- 208000019206 urinary tract infection Diseases 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/84—Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Cephalosporin Compounds (AREA)
Abstract
The invention discloses a method for recovering N, N' -dibenzylethylenediamine salt from ion exchange resin to be regenerated of cefonicid sodium, belonging to the technical field of medicines and comprising the following steps: weighing a certain amount of ion exchange resin to be regenerated of cefonicid sodium, adding an alkaline solution, stirring, and filtering to obtain a filtrate; b, carrying out rotary evaporation on the filtrate under reduced pressure to obtain solid residues, adding ethyl acetate into the solid residues, and stirring and dissolving to obtain a dissolved solution; c, adding saline water into the dissolved solution, and carrying out extraction phase separation; d, adding a drying agent into the obtained organic phase, and filtering the organic phase into a crystallizer; e, adding an acidic reagent, a crystallization agent and seed crystals into the crystallizer for growing crystals; and f, after the crystal growth is finished, carrying out suction filtration treatment to obtain a filter cake, washing the filter cake, and then carrying out vacuum drying to obtain the N, N' -dibenzylethylenediamine salt. The method has the advantages of stable quality of recovered products, simple recovery method and high recovery rate, and reduces COD discharged by the mother liquor.
Description
Technical Field
The invention relates to the technical field of medicines, in particular to a method for recovering N, N' -dibenzylethylenediamine salt.
Background
Cefonicid sodium is the second generation cephalosporin, generates antibacterial activity by inhibiting bacterial cell wall synthesis, has antibacterial effect on gram positive and negative bacteria and some anaerobes, is stable to most of beta-lactamase, is suitable for lower respiratory tract infection, urinary tract infection, septicemia, skin soft tissue infection, bone and joint infection caused by sensitive bacteria, and can also be used for operation infection prevention. The product is white or quasi-white powder or crystalline powder. The product is very soluble in water, slightly soluble in methanol, very slightly soluble in ethanol, and hardly soluble in diethyl ether. The chemical name is as follows: (6R,7R) -7- [ (R) - α -hydroxyphenylacetamido ] -8-oxo-3- [ [ [ 1-sulfomethyl-1H-tetrazol-5-yl ] thio ] methyl ] -5-thia-1-azabicyclo [4.2.0] oct-2-ene-2-carboxylic acid disodium salt. The structural formula is as follows:
in the production process, the ion exchange resin needs to be activated and regenerated after being used up each time, and the eluted N, N' -dibenzyl ethylenediamine is directly discharged to a sewage tank without being recovered, so that the environmental impact is large.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for recovering N, N' -dibenzylethylenediamine salt from an ion exchange resin to be regenerated of cefonicid sodium, which has the advantages of stable quality of recovered products, simple recovery method and high recovery rate, and reduces COD (chemical oxygen demand) discharged by mother liquor.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for recovering N, N' -dibenzyl ethylenediamine salt from an ion exchange resin to be regenerated of cefonicid sodium is characterized by comprising the following steps:
weighing a certain amount of ion exchange resin to be regenerated of cefonicid sodium, adding an alkaline solution into the ion exchange resin, stirring, and filtering to obtain a filtrate;
b, carrying out rotary evaporation on the filtrate under reduced pressure to obtain solid residues, adding ethyl acetate into the solid residues, and stirring and dissolving to obtain a dissolved solution;
c, adding saline water into the dissolved solution, and performing extraction phase separation;
d, adding a drying agent into the organic phase obtained by phase separation, and filtering the mixture into a crystallizer;
e, adding an acidic reagent, a crystallization agent and seed crystals into the crystallizer for growing crystals;
and f, after the crystal growth is finished, carrying out suction filtration treatment to obtain a filter cake, washing the filter cake, and then carrying out vacuum drying to obtain the N, N' -dibenzylethylenediamine salt.
The technical scheme of the invention is further improved as follows: the alkaline solution added in the step a is a methanol solution containing 10% of sodium hydroxide or 10% of potassium hydroxide, and the weight volume ratio (kg/L) of the ion exchange resin to the alkaline solution is 1.
The technical scheme of the invention is further improved as follows: and d, adding saline water into the solution, stirring for 0.5-1 hour, standing for 0.5-1 hour, and performing phase separation.
The technical scheme of the invention is further improved as follows: the volume ratio (L/L/L) of the dosage of the alkaline solution, the dosage of the ethyl acetate and the dosage of the saline is 1 (2-5) to 2.
The technical scheme of the invention is further improved as follows: the drying agent is anhydrous magnesium sulfate or anhydrous sodium sulfate, the drying time is 1 hour, and the dosage of the drying agent is 10 percent of the weight of the resin.
The technical scheme of the invention is further improved as follows: the acidic reagent in the step e is glacial acetic acid, the crystallization agent is ethyl acetate, and the volume ratio (L/L/L) of the dosage of the acidic reagent, the dosage of the crystallization agent and the dosage of the saline water is 1 (10-20): (20-50).
The technical scheme of the invention is further improved as follows: the dosage of the seed crystal in the step e is 2 percent of the weight of the resin; the temperature of growing the crystal is 5-10 ℃, and the time of growing the crystal is 1-2 hours.
Due to the adoption of the technical scheme, the invention has the technical progress that:
the invention can obtain the N, N' -dibenzylethylenediamine salt product with higher purity by eluting, extracting and crystallizing the ion exchange resin to be regenerated of the cefonicid sodium, has the advantages of stable quality of recovered products, simple recovery method and high recovery rate, and simultaneously reduces COD (chemical oxygen demand) discharged by mother liquor and lightens the pollution to the environment.
Detailed Description
The present invention is further illustrated in detail below with reference to examples:
a method for recovering N, N' -dibenzyl ethylenediamine salt from an ion exchange resin to be regenerated of cefonicid sodium comprises the following steps:
a, weighing a certain amount of ion exchange resin to be regenerated of cefonicid sodium, adding an alkaline solution into the ion exchange resin, stirring, and filtering to obtain a filtrate;
b, carrying out rotary evaporation on the filtrate under reduced pressure to obtain a solid residue, adding ethyl acetate into the solid residue, and stirring for dissolving to obtain a dissolved solution;
c, adding saline water into the dissolved solution, and carrying out extraction phase separation;
d, adding a drying agent into the organic phase obtained by phase separation, and filtering the mixture into a crystallizer;
e, adding an acidic reagent, a crystallization agent and seed crystals into the crystallizer for crystal growing;
and f, after the crystal growing is finished, carrying out suction filtration treatment to obtain a filter cake, washing the filter cake, and then carrying out vacuum drying to obtain the N, N' -dibenzylethylenediamine salt.
The method comprises the following steps of (1) adding an alkaline solution into a methanol solution containing 10% of sodium hydroxide or 10% of potassium hydroxide, adding brine into a saturated sodium chloride solution, adding an acidic reagent into glacial acetic acid, adding a crystallization agent into ethyl acetate, adding a drying agent into anhydrous magnesium sulfate or anhydrous sodium sulfate, wherein the weight volume ratio (kg/L) of ion exchange resin to the alkaline solution is 1 to 2-1: (20-50).
Wherein, in the step c, the brine is added into the dissolved solution, then the solution is stirred for 0.5 to 1 hour, and the solution is kept stand for 0.5 to 1 hour and then phase splitting is carried out; in the step d, the drying time is 1 hour, and the using amount of the drying agent is 10 percent of the weight of the resin; the dosage of the seed crystal in the step e is 2 percent of the weight of the resin, the crystal growing temperature is 5 to 10 ℃, and the crystal growing time is 1 to 2 hours.
Example 1
Taking 20g of ion exchange resin to be regenerated, washing the resin with 40mL of 10% sodium hydroxide methanol solution, stirring for 0.5 h, filtering the resin, and spin-drying the filtrate at 40 ℃.
Adding 80mL of ethyl acetate to dissolve, adding 80mL of saturated sodium chloride after the solution is clear, stirring for 0.5 hour, standing for 0.5 hour, and separating to obtain an organic phase.
Drying with 2g anhydrous magnesium sulfate for 1h, filtering to crystallizer, adding 4mL glacial acetic acid, 40mL ethyl acetate, 0.4g seed crystal, growing crystal at 5 deg.C for 1 h.
Filtering; after the crystal growth is finished, carrying out suction filtration treatment to obtain a filter cake, soaking and washing the filter cake for 1 time by using 50mL ethyl acetate, and carrying out vacuum drying at 50 ℃ until the quality requirement is met; 10.67g of white crystals were obtained with a purity of 99.2%.
Example 2
Taking 20g of ion exchange resin to be regenerated, washing the resin by using 100mL of 10% sodium hydroxide methanol solution, stirring for 1 hour, filtering the resin, and spin-drying the filtrate at 40 ℃.
Adding 500mL of ethyl acetate to dissolve, adding 200mL of saturated sodium chloride after dissolving, stirring for 1 hour, standing for 1 hour, and separating to obtain an organic phase.
Drying with 2g anhydrous magnesium sulfate for 1h, filtering to crystallizer, adding 4mL glacial acetic acid, 80mL ethyl acetate, 0.4g seed crystal, growing crystal at 10 deg.C for 2 h.
Filtering; after the crystal growth is finished, carrying out suction filtration treatment to obtain a filter cake, soaking and washing the filter cake for 1 time by using 50mL ethyl acetate, and carrying out vacuum drying at 50 ℃ until the quality requirement is met; 11.67g of white crystals were obtained with a purity of 99.4%.
Example 3
Taking 20g of ion exchange resin to be regenerated, washing the resin with 60mL of 10% potassium hydroxide methanol solution, stirring for 0.5 h, filtering the resin, and spin-drying the filtrate at 40 ℃.
Adding 180mL of ethyl acetate to dissolve, adding 120mL of saturated sodium chloride after dissolving, stirring for 0.6 hour, standing for 0.6 hour, and separating to obtain an organic phase.
Drying with 2g anhydrous magnesium sulfate for 1h, filtering to crystallizer, adding 4mL glacial acetic acid, 60mL ethyl acetate, 0.4g seed crystal, growing crystal at 8 deg.C for 1 h.
Filtering; after the crystal growth is finished, carrying out suction filtration treatment to obtain a filter cake, soaking and washing the filter cake for 1 time by using 50mL ethyl acetate, and carrying out vacuum drying at 50 ℃ until the quality requirement is met; 11.97g of white crystals were obtained with a purity of 99.5%.
Table 1: quality tests were performed on 3 samples of the examples, with the following data:
| detecting items | Internal control standard of enterprise | Commercially available 1 | Example 1 | Example 2 | Example 3 |
| Moisture content | ≤0.5％ | 0.14 | 0.10 | 0.07 | 0.09 |
| Content (c) of | 99.0-101.0％ | 99.8 | 99.8 | 99.9 | 99.7 |
| Acidity of | 5.0-6.0 | 5.4 | 5.5 | 5.6 | 5.5 |
| Color of solution | Number 3 or less | < number 2 | < No. 1 | < number 1 | < number 1 |
According to the data in Table 1, the purity index of the recovered product is equivalent to that of the commercial product, the color grade level is superior to that of the commercial product, the recovery process is stable, and the reproducibility is good.
Table 2: EXAMPLE 1-3 recovery of cefonicid sodium for use with commercial products to prepare cefonicid sodium quality Scale
According to the data in table 2, the quality of the recovered cefonicid sodium product meets the pharmacopeia standard, and the cefonicid sodium product prepared from the recovered dibenzylethylenediamine salt has obvious advantages in color grade level.
The method of the invention recovers N, N' -dibenzylethylenediamine salt from cefonicid sodium resin, and the prepared cefonicid sodium has certain advantages in color grade indexes; the recovery process is stable, the production cost is effectively reduced, the COD discharged by the mother liquor is reduced, the process is simple to operate, and the process is suitable for industrialization.
Claims (7)
1. A method for recovering N, N' -dibenzyl ethylenediamine salt from an ion exchange resin to be regenerated of cefonicid sodium is characterized by comprising the following steps:
weighing a certain amount of ion exchange resin to be regenerated of cefonicid sodium, adding an alkaline solution into the ion exchange resin, stirring, and filtering to obtain a filtrate;
b, carrying out rotary evaporation on the filtrate under reduced pressure to obtain solid residues, adding ethyl acetate into the solid residues, and stirring and dissolving to obtain a dissolved solution;
c, adding saline water into the dissolved solution, and performing extraction phase separation, wherein the saline water is a saturated sodium chloride solution;
d, adding a drying agent into the organic phase obtained by phase separation, and filtering the mixture into a crystallizer;
e, adding an acidic reagent, a crystallization agent and seed crystals into the crystallizer for crystal growing;
and f, after the crystal growth is finished, carrying out suction filtration treatment to obtain a filter cake, washing the filter cake, and then carrying out vacuum drying to obtain the N, N' -dibenzylethylenediamine salt.
2. The process of claim 1 for recovering N, N' -dibenzylethylenediamine salt from an ion exchange resin to be regenerated from cefonicid sodium, characterized by: the alkaline solution added in the step a is a methanol solution containing 10% of sodium hydroxide or 10% of potassium hydroxide, the weight volume ratio of the ion exchange resin to the alkaline solution is 1.
3. The process of claim 2 for recovering benzathine salt from the ion exchange resin to be regenerated of cefonicid sodium, characterized by: and c, adding the saline water into the dissolved solution in the step c, stirring for 0.5-1 hour, standing for 0.5-1 hour, and then carrying out phase separation.
4. The process of claim 3 for the recovery of benzathine salt from ion exchange resin to be regenerated comprising the steps of: the ratio of the dosage volume of the alkaline solution to the dosage volume of the ethyl acetate to the dosage volume of the saline is 1 (2-5) to 2, wherein the volume units are L.
5. The process of claim 1 for recovering N, N' -dibenzylethylenediamine salt from an ion exchange resin to be regenerated from cefonicid sodium, characterized by: the drying agent is anhydrous magnesium sulfate or anhydrous sodium sulfate, the drying time is 1 hour, and the dosage of the drying agent is 10 percent of the weight of the resin.
6. The process of claim 3 for the recovery of benzathine salt from ion exchange resin to be regenerated comprising the steps of: the acidic reagent in the step e is glacial acetic acid, the crystallization agent is ethyl acetate, and the ratio of the dosage volume of the acidic reagent to the dosage volume of the crystallization agent to the dosage volume of the saline water is 1 (10-20): (20-50), wherein the volume units are L.
7. The process of claim 1 for recovering benzathine salt from the ion exchange resin to be regenerated comprising cefonicid sodium, wherein: the dosage of the seed crystal in the step e is 2 percent of the weight of the resin; the temperature of growing the crystal is 5-10 ℃, and the time of growing the crystal is 1-2 hours.
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| CN201911073832.5A CN111072497B (en) | 2019-11-06 | 2019-11-06 | Method for recovering N, N' -dibenzylethylenediamine salt from ion exchange resin to be regenerated of cefonicid sodium |
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| CN201911073832.5A CN111072497B (en) | 2019-11-06 | 2019-11-06 | Method for recovering N, N' -dibenzylethylenediamine salt from ion exchange resin to be regenerated of cefonicid sodium |
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| CN109232610A (en) * | 2018-09-04 | 2019-01-18 | 华北制药河北华民药业有限责任公司 | A kind of refining methd of cefonicid dibenzylethylenediamsalt salt |
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| CN109232610A (en) * | 2018-09-04 | 2019-01-18 | 华北制药河北华民药业有限责任公司 | A kind of refining methd of cefonicid dibenzylethylenediamsalt salt |
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| Title |
|---|
| 头孢尼西钠制备工艺研究;胡利敏 等;《化工管理》;20180221(第6期);第91-92页 * |
| 头孢尼西钠的合成;李凤侠 等;《山东化工》;20181015;第37卷(第10期);第10-11页 * |
| 头孢尼西钠的合成方法改进;魏青杰 等;《中国新药杂志》;20120330;第21卷(第6期);第690-692页 * |
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