CN105884697A - Method for preparing sulfadimidine salt - Google Patents
Method for preparing sulfadimidine salt Download PDFInfo
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- CN105884697A CN105884697A CN201410698041.2A CN201410698041A CN105884697A CN 105884697 A CN105884697 A CN 105884697A CN 201410698041 A CN201410698041 A CN 201410698041A CN 105884697 A CN105884697 A CN 105884697A
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- sulfadimidine
- ethanol
- methanol
- filter cake
- isopropanol
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Abstract
The invention discloses a method for preparing a sulfadimidine salt. The method comprises the following steps: dissolving, washing, crystallizing and drying. According to the method, water serves as a solvent, the toxicity of water is nearly zero, and the headache possibility of a patient is reduced.
Description
Technical field
The present invention relates to the preparation method of a kind of pharmaceutical product containing organic effective component containing the compound to benzene sulfonyl N base having 1 heterocycle,
A kind of preparation method of sulfadimidine salt.
Background technology
Sulfadimidine, Chinese is N-(4,6-dimethyl-2-pyrimidine radicals)-4-aminobenzenesul fonamide, and English name is
Sulfamethazinum, English is abbreviated as SM2, for white or yellowish crystallization or powder, odorless, mildly bitter flavor, meets photochromic gradual change deep, in heat
Ethanol dissolves, insoluble in water or ether, readily soluble in olefin(e) acid or dilute alkaline soln, for disulfonamide, it is adaptable to treatment Hemolytic streptococcus,
Meningococcus, streptococcus pneumoniae etc. catch, lasting medicine, have that antibiotic property is strong, toxicity is little, infiltration rate is complete.
Sulfadimidine is the most insoluble in water, during use, needs to use the organic solvents such as ethanol to use, and alcohol toxicity belongs to micro-toxicity,
The ill symptomses such as headache can be caused.
Summary of the invention
For the defect of above-mentioned prior art, the invention provides the preparation method of a kind of sulfadimidine salt, it is adopted and uses water as solvent, water
Toxicity is almost nil, reduces the headache probability of patient.
In order to reach above-mentioned advantage, the present invention specifically have employed following technical scheme.
A kind of preparation method of sulfadimidine salt, its step includes:
1) dissolving step: add sulfuric acid mixture liquid in dissolving tank at 25 ± 5 DEG C, be subsequently adding the sulfadimidine of 1 weight portion, 0.01～0.02
The sodium sulfite of weight portion and the aqueous solution of 0.1～0.2 parts by volume, stir 20～30min, filters, obtains solution A；Described sulfuric acid mixture liquid
Preparation method be in dissolving tank, to add a kind of solvent in ethanol, methanol or isopropanol, stirring, at 40 DEG C, drip sulphuric acid, ethanol/methanol/different
Propanol: sulfadimidine=4.0～8.0: 1, sulphuric acid: sulfadimidine=0.25～0.40: 1；
2) crystallisation step: solution A is placed in crystallizer, in 35 ± 5 DEG C of stirring and crystallizing, is cooled to 0～10 DEG C, continues stirring 2 hours, obtains
Mixed liquid B；
3) washing step: filter mixed liquor B, with solvent washing filter cake a kind of in ethanol, methanol or isopropanol, takes filter cake C；
4) drying steps: at 40～50 DEG C, filter cake C is dried under vacuum to moisture content≤5.5%, obtains sulfadimidine hydrosulfate dry powder D.
Advantages of the present invention is, adopts and uses water as solvent, and the toxicity of water is almost nil, reduces the headache probability of patient.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further details.
Embodiment 1
A kind of preparation method of sulfadimidine salt, its step includes:
1) dissolving step: add sulfuric acid mixture liquid in dissolving tank at 25 ± 5 DEG C, be subsequently adding the sulfadimidine of 1 weight portion, 0.01 weight
The sodium sulfite of amount part and the aqueous solution of 0.1 parts by volume, stir 20min, filters, obtains solution A；The preparation method of described sulfuric acid mixture liquid
For, dissolving tank adds a kind of solvent in ethanol, methanol or isopropanol, stirring, at 40 DEG C, drips sulphuric acid, ethanol/methanol/isopropanol: sulfanilamide
Diformazan pyrimidine=4.0～8.0: 1, sulphuric acid: sulfadimidine=0.25: 1；
2) crystallisation step: solution A is placed in crystallizer, in 35 ± 5 DEG C of stirring and crystallizing, is cooled to 0 DEG C, continues stirring 2 hours, is mixed
Liquid B；
3) washing step: filter mixed liquor B, with solvent washing filter cake a kind of in ethanol, methanol or isopropanol, takes filter cake C；
4) drying steps: at 40 DEG C, filter cake C is dried under vacuum to moisture content≤5.5%, obtains sulfadimidine hydrosulfate dry powder D.
Embodiment 2
A kind of preparation method of sulfadimidine salt, its step includes:
1) dissolving step: add sulfuric acid mixture liquid in dissolving tank at 25 ± 5 DEG C, be subsequently adding the sulfadimidine of 1 weight portion, 0.02 weight
The sodium sulfite of amount part and the aqueous solution of 0.2 parts by volume, stir 30min, filters, obtains solution A；The preparation method of described sulfuric acid mixture liquid
For, dissolving tank adds a kind of solvent in ethanol, methanol or isopropanol, stirring, at 40 DEG C, drips sulphuric acid, ethanol/methanol/isopropanol: sulfanilamide
Diformazan pyrimidine=8.0: 1, sulphuric acid: sulfadimidine=0.40: 1；
2) crystallisation step: solution A is placed in crystallizer, in 35 ± 5 DEG C of stirring and crystallizing, is cooled to 10 DEG C, continues stirring 2 hours, is mixed
Close liquid B；
3) washing step: filter mixed liquor B, with solvent washing filter cake a kind of in ethanol, methanol or isopropanol, takes filter cake C；
4) drying steps: at 50 DEG C, filter cake C is dried under vacuum to moisture content≤5.5%, obtains sulfadimidine hydrosulfate dry powder D.
Embodiment 3
A kind of preparation method of sulfadimidine salt, its step includes:
1) dissolving step: add sulfuric acid mixture liquid in dissolving tank at 25 ± 5 DEG C, be subsequently adding the sulfadimidine of 1 weight portion, 0.013 weight
The sodium sulfite of amount part and the aqueous solution of 0.13 parts by volume, stir 22min, filters, obtains solution A；The preparation method of described sulfuric acid mixture liquid
For, dissolving tank adds a kind of solvent in ethanol, methanol or isopropanol, stirring, at 40 DEG C, drips sulphuric acid, ethanol/methanol/isopropanol: sulfanilamide
Diformazan pyrimidine=5.0: 1, sulphuric acid: sulfadimidine=0.27: 1；
2) crystallisation step: solution A is placed in crystallizer, in 35 ± 5 DEG C of stirring and crystallizing, is cooled to 2 DEG C, continues stirring 2 hours, is mixed
Liquid B；
3) washing step: filter mixed liquor B, with solvent washing filter cake a kind of in ethanol, methanol or isopropanol, takes filter cake C；
4) drying steps: at 42 DEG C, filter cake C is dried under vacuum to moisture content≤5.5%, obtains sulfadimidine hydrosulfate dry powder D.
Embodiment 4
A kind of preparation method of sulfadimidine salt, its step includes:
1) dissolving step: add sulfuric acid mixture liquid in dissolving tank at 25 ± 5 DEG C, be subsequently adding the sulfadimidine of 1 weight portion, 0.015 weight
The sodium sulfite of amount part and the aqueous solution of 0.15 parts by volume, stir 23min, filters, obtains solution A；The preparation method of described sulfuric acid mixture liquid
For, dissolving tank adds a kind of solvent in ethanol, methanol or isopropanol, stirring, at 40 DEG C, drips sulphuric acid, ethanol/methanol/isopropanol: sulfanilamide
Diformazan pyrimidine=6.0: 1, sulphuric acid: sulfadimidine=0.3: 1；
2) crystallisation step: solution A is placed in crystallizer, in 35 ± 5 DEG C of stirring and crystallizing, is cooled to 4 DEG C, continues stirring 2 hours, is mixed
Liquid B；
3) washing step: filter mixed liquor B, with solvent washing filter cake a kind of in ethanol, methanol or isopropanol, takes filter cake C；
4) drying steps: at 44 DEG C, filter cake C is dried under vacuum to moisture content≤5.5%, obtains sulfadimidine hydrosulfate dry powder D.
Embodiment 5
A kind of preparation method of sulfadimidine salt, its step includes:
1) dissolving step: add sulfuric acid mixture liquid in dissolving tank at 25 ± 5 DEG C, be subsequently adding the sulfadimidine of 1 weight portion, 0.017 weight
The sodium sulfite of amount part and the aqueous solution of 0.17 parts by volume, stir 25min, filters, obtains solution A；The preparation method of described sulfuric acid mixture liquid
For, dissolving tank adds a kind of solvent in ethanol, methanol or isopropanol, stirring, at 40 DEG C, drips sulphuric acid, ethanol/methanol/isopropanol: sulfanilamide
Diformazan pyrimidine=7.0: 1, sulphuric acid: sulfadimidine=0.25～0.40: 1；
2) crystallisation step: solution A is placed in crystallizer, in 35 ± 5 DEG C of stirring and crystallizing, is cooled to 6 DEG C, continues stirring 2 hours, is mixed
Liquid B；
3) washing step: filter mixed liquor B, with solvent washing filter cake a kind of in ethanol, methanol or isopropanol, takes filter cake C；
4) drying steps: at 46 DEG C, filter cake C is dried under vacuum to moisture content≤5.5%, obtains sulfadimidine hydrosulfate dry powder D.
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, and is not the limit to embodiment of the present invention
Fixed.For the technical staff in described field, can also make other changes in different forms on the basis of the above description.Here without
Need also to give exhaustive to all of embodiment.And these spirit belonging to the present invention are amplified out obvious change or variation still in
Among protection scope of the present invention.
Claims (3)
1. the preparation method of a sulfadimidine salt, it is characterised in that its step includes:
1) dissolving step: add sulfuric acid mixture liquid in dissolving tank at 25 ± 5 DEG C, be subsequently adding the sulfadimidine of 1 weight portion, 0.01～0.02
The sodium sulfite of weight portion and the aqueous solution of 0.1～0.2 parts by volume, stir 20～30min, filters, obtains solution A；Described sulfuric acid mixture liquid
Preparation method be in dissolving tank, to add a kind of solvent in ethanol, methanol or isopropanol, stirring, at 40 DEG C, drip sulphuric acid, ethanol/methanol/different
Propanol: sulfadimidine=4.0～8.0: 1, sulphuric acid: sulfadimidine=0.25～0.40: 1；
2) crystallisation step: solution A is placed in crystallizer, in 35 ± 5 DEG C of stirring and crystallizing, is cooled to 0～10 DEG C, continues stirring 2 hours, obtains
Mixed liquid B；
3) washing step: filter mixed liquor B, with solvent washing filter cake a kind of in ethanol, methanol or isopropanol, takes filter cake C；
4) drying steps: at 40～50 DEG C, filter cake C is dried under vacuum to moisture content≤5.5%, obtains sulfadimidine hydrosulfate dry powder D.
2. the preparation method of sulfadimidine salt as claimed in claim 1, it is characterised in that its step includes:
1) dissolving step: add sulfuric acid mixture liquid in dissolving tank at 25 ± 5 DEG C, be subsequently adding the sulfadimidine of 1 weight portion, 0.01 weight
The sodium sulfite of amount part and the aqueous solution of 0.1 parts by volume, stir 20min, filters, obtains solution A；The preparation method of described sulfuric acid mixture liquid
For, dissolving tank adds a kind of solvent in ethanol, methanol or isopropanol, stirring, at 40 DEG C, drips sulphuric acid, ethanol/methanol/isopropanol: sulfanilamide
Diformazan pyrimidine=4.0: 1, sulphuric acid: sulfadimidine=0.25: 1；
2) crystallisation step: solution A is placed in crystallizer, in 35 ± 5 DEG C of stirring and crystallizing, is cooled to 0 DEG C, continues stirring 2 hours, is mixed
Liquid B；
3) washing step: filter mixed liquor B, with solvent washing filter cake a kind of in ethanol, methanol or isopropanol, takes filter cake C；
4) drying steps: at 40 DEG C, filter cake C is dried under vacuum to moisture content≤5.5%, obtains sulfadimidine hydrosulfate dry powder D.
3. the preparation method of sulfadimidine salt as claimed in claim 1, it is characterised in that its step includes:
1) dissolving step: add sulfuric acid mixture liquid in dissolving tank at 25 ± 5 DEG C, be subsequently adding the sulfadimidine of 1 weight portion, 0.02 weight
The sodium sulfite of amount part and the aqueous solution of 0.2 parts by volume, stir 30min, filters, obtains solution A；The preparation method of described sulfuric acid mixture liquid
For, dissolving tank adds a kind of solvent in ethanol, methanol or isopropanol, stirring, at 40 DEG C, drips sulphuric acid, ethanol/methanol/isopropanol: sulfanilamide
Diformazan pyrimidine=8.0: 1, sulphuric acid: sulfadimidine=0.40: 1；
2) crystallisation step: solution A is placed in crystallizer, in 35 ± 5 DEG C of stirring and crystallizing, is cooled to 10 DEG C, continues stirring 2 hours, is mixed
Close liquid B；
3) washing step: filter mixed liquor B, with solvent washing filter cake a kind of in ethanol, methanol or isopropanol, takes filter cake C；
4) drying steps: at 50 DEG C, filter cake C is dried under vacuum to moisture content≤5.5%, obtains sulfadimidine hydrosulfate dry powder D.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410698041.2A CN105884697A (en) | 2014-11-28 | 2014-11-28 | Method for preparing sulfadimidine salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410698041.2A CN105884697A (en) | 2014-11-28 | 2014-11-28 | Method for preparing sulfadimidine salt |
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| CN105884697A true CN105884697A (en) | 2016-08-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410698041.2A Pending CN105884697A (en) | 2014-11-28 | 2014-11-28 | Method for preparing sulfadimidine salt |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1217936A (en) * | 1967-07-20 | 1971-01-06 | American Cyanamid Co | Water-soluble sulfonamide and tetracycline acid salt compositions |
| CN103709109A (en) * | 2013-12-24 | 2014-04-09 | 福建省福抗药业股份有限公司 | Preparation method of sulfadimidine hydrosulfate |
-
2014
- 2014-11-28 CN CN201410698041.2A patent/CN105884697A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1217936A (en) * | 1967-07-20 | 1971-01-06 | American Cyanamid Co | Water-soluble sulfonamide and tetracycline acid salt compositions |
| CN103709109A (en) * | 2013-12-24 | 2014-04-09 | 福建省福抗药业股份有限公司 | Preparation method of sulfadimidine hydrosulfate |
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Application publication date: 20160824 |