CN109134387A - A kind of preparation method of Sulfamonomethoxime Sodium and Sulfamonomethoxime Sodium prepared by this method - Google Patents
A kind of preparation method of Sulfamonomethoxime Sodium and Sulfamonomethoxime Sodium prepared by this method Download PDFInfo
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- CN109134387A CN109134387A CN201710464902.4A CN201710464902A CN109134387A CN 109134387 A CN109134387 A CN 109134387A CN 201710464902 A CN201710464902 A CN 201710464902A CN 109134387 A CN109134387 A CN 109134387A
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- sulfamonomethoxime
- sulfamonomethoxime sodium
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
- C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
- C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
- C07D239/69—Benzenesulfonamido-pyrimidines
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Abstract
The present invention provides a kind of preparation method of Sulfamonomethoxime Sodium, and the preparation method of Sulfamonomethoxime Sodium provided by the present invention, production process alkali wasteliquid is few, and waste liquid is almost neutrality, high income, product purity height.Sulfamonomethoxime Sodium made from this method is easily separated with solvent, and product purity is high, high income, is suitable for industrialized production.
Description
Technical field
The present invention relates to the preparation method of veterinary drug technology of preparing more particularly to a kind of Sulfamonomethoxime Sodium and thus side
The Sulfamonomethoxime Sodium of method preparation.
Background technique
Sulfamonomethoxime Sodium is the strongest sulfa drug of antibertisis in vivo and in vitro, to most of gram-positive bacterias and yin
Property bacterium have compared with high inhibition act on, bacterium to this medicine generate drug resistance it is slower.It is mainly used for sensitive bacteria, toxoplasm, eperytozoa
Various diseases and its mixed infection caused by body.
Preparing Sulfamonomethoxime Sodium common method at present is that oxygen pyrimidine is reacted with sodium hydroxide solution between sulfanilamide (SN), instead
It answers liquid to be decolourized, filters, dry obtained Sulfamonomethoxime Sodium.The alkali wasteliquid amount that this method generates is big, and yield is low, product
Impurity content is high.
Summary of the invention
To solve the above problems, the present invention provides a kind of preparation method of Sulfamonomethoxime Sodium, preparation process alkali is useless
Liquid is few, high income, and product purity is high.
The technical solution of the present invention is as follows: a kind of preparation method of Sulfamonomethoxime Sodium and sulfanilamide (SN) prepared by this method
Between Sulfamonomethoxine sodium, comprising the following steps:
(1) daimeton, sodium hydroxide are added in organic solvent, under the conditions of 54 ~ 98 DEG C of temperature, are stirred to react
0.5-2 hours, obtain solution A；
(2) active carbon is added to solution A, stirring decoloration 0.3-0.8 hours filters while hot, obtains filtrate；
(3) filtrate first naturally cools to 20 ~ 30 DEG C, then at 0 ~ 5 DEG C, keeps the temperature 1-3 hours, and filtering obtains filter residue；
(4) wash filter residue with a small amount of dehydrated alcohol, 55 ~ 60 DEG C vacuum drying 2-4 hours, obtain Sulfamonomethoxime Sodium.
In the step (1), the mass ratio of daimeton and sodium hydroxide is 1:(0.13 ~ 0.15).
In the step (1), the mass ratio of daimeton and sodium hydroxide is 1:0.14.
In the step (1), the mass volume ratio of daimeton and organic solvent is 1:(8.5 ~ 15), unit is
g/ml。
In the step (1), the mass volume ratio of daimeton and organic solvent is 1:10, unit g/ml.
In the step (1), used organic solvent is ethyl alcohol.
In the step (2), the volume mass ratio of active carbon and organic solution is 0.3:100, unit g/ml.
The Sulfamonomethoxime Sodium of the preparation method preparation of above-mentioned Sulfamonomethoxime Sodium.
Beneficial effects of the present invention: the preparation method of Sulfamonomethoxime Sodium provided by the present invention, production process alkali
Waste liquid is few, and waste liquid is almost neutrality, high income, product purity height.Sulfamonomethoxime Sodium made from this method is easily and solvent
Separation, product purity is high, high income, is suitable for industrialized production.
Specific embodiment
Embodiment 1
A kind of preparation method of Sulfamonomethoxime Sodium, comprising the following steps:
(1) daimeton, sodium hydroxide are added in organic solvent, under the conditions of 54 ~ 98 DEG C of temperature, are stirred to react
0.5-2 hours, obtain solution A；
(2) active carbon is added to solution A, stirring decoloration 0.3-0.8 hours filters while hot, obtains filtrate；
(3) filtrate first naturally cools to 20 ~ 30 DEG C, then at 0 ~ 5 DEG C, keeps the temperature 1-3 hours, and filtering obtains filter residue；
(4) wash filter residue with a small amount of dehydrated alcohol, 55 ~ 60 DEG C vacuum drying 2-4 hours, obtain Sulfamonomethoxime Sodium.
Embodiment 2
A kind of preparation method of Sulfamonomethoxime Sodium, comprising the following steps:
(1) daimeton, sodium hydroxide are added in organic solvent, under the conditions of 54 ~ 98 DEG C of temperature, are stirred to react 1
Hour, obtain solution A；
(2) active carbon is added to solution A, stirring decoloration 0.5 hour filters while hot, obtains filtrate；
(3) filtrate first naturally cools to 20 ~ 30 DEG C, then at 0 ~ 5 DEG C, keeps the temperature 2 hours, and filtering obtains filter residue；
(4) filter residue is washed with a small amount of dehydrated alcohol, is dried in vacuo 3 hours at 55 ~ 60 DEG C, obtains Sulfamonomethoxime Sodium.
Embodiment 3
A kind of preparation method of Sulfamonomethoxime Sodium, comprising the following steps:
By 20g daimeton, 2.8g sodium hydroxide is added in 200ml ethyl alcohol, under the conditions of 70 ~ 82 DEG C of temperature, stirring
0.6g active carbon is added in reaction 1 hour, and stirring decoloration 0.5 hour is filtered while hot, and filtrate first naturally cools to 20 ~ 30 DEG C, then
At 0 ~ 5 DEG C, keep the temperature 2 hours, filtering, washed with a small amount of dehydrated alcohol it is colourless to cleaning solution, it is 3 small in 55 ~ 60 DEG C of vacuum drying
When, obtain Sulfamonomethoxime Sodium 20.92g, yield 96.97%.Sulfamonomethoxime Sodium is white crystalline powder, pure
Degree is 99.4%.Waste liquid weakly acidic pH is filtered during the preparation process.
Embodiment 4
A kind of preparation method of Sulfamonomethoxime Sodium, comprising the following steps:
By 20g daimeton, 2.8g sodium hydroxide is added in 200ml methanol, under the conditions of 60 ~ 68 DEG C of temperature, stirring
0.6g active carbon is added in reaction 1 hour, and stirring decoloration 0.5 hour is filtered while hot, and filtrate first naturally cools to 20 ~ 30 DEG C, then
At 0 ~ 5 DEG C, keep the temperature 2 hours, filtering, washed with a small amount of dehydrated alcohol it is colourless to cleaning solution, it is 3 small in 55 ~ 60 DEG C of vacuum drying
When, obtain Sulfamonomethoxime Sodium 19.84g, yield 91.98%.Sulfamonomethoxime Sodium is white crystalline powder, pure
Degree is 99.1%.Waste liquid weakly acidic pH is filtered during the preparation process.
Embodiment 5
A kind of preparation method of Sulfamonomethoxime Sodium, comprising the following steps:
By 20g daimeton, 2.8g sodium hydroxide is added in 200ml normal propyl alcohol, under the conditions of 95 ~ 98 DEG C of temperature, stirs
Reaction 1 hour to be mixed, 0.6g active carbon is added, stirring decoloration 0.5 hour is filtered while hot, and filtrate first naturally cools to 20 ~ 30 DEG C,
Again at 0 ~ 5 DEG C, keep the temperature 2 hours, filtering, washed with a small amount of dehydrated alcohol it is colourless to cleaning solution, 55 ~ 60 DEG C be dried in vacuo 3
Hour, obtain Sulfamonomethoxime Sodium 20.22g, yield 93.74%.Sulfamonomethoxime Sodium is white crystalline powder,
Purity is 99.2%.Waste liquid weakly acidic pH is filtered during the preparation process.
Embodiment 6
A kind of preparation method of Sulfamonomethoxime Sodium, comprising the following steps:
By 20g daimeton, 2.8g sodium hydroxide is added in 200ml acetone, under the conditions of 53 ~ 58 DEG C of temperature, stirring
0.6g active carbon is added in reaction 1 hour, and stirring decoloration 0.5 hour is filtered while hot, and filtrate first naturally cools to 20 ~ 30 DEG C, then
At 0 ~ 5 DEG C, keep the temperature 2 hours, filtering, washed with a small amount of dehydrated alcohol it is colourless to cleaning solution, it is 3 small in 55 ~ 60 DEG C of vacuum drying
When, obtain Sulfamonomethoxime Sodium 19.92g, yield 92.35%.Sulfamonomethoxime Sodium is white crystalline powder, pure
Degree is 99.5%.Waste liquid weakly acidic pH is filtered during the preparation process.
Embodiment 7
A kind of preparation method of Sulfamonomethoxime Sodium, comprising the following steps:
By 20g daimeton, 2.6g sodium hydroxide is added in 170ml ethyl alcohol, under the conditions of 70 ~ 82 DEG C of temperature, stirring
0.51g active carbon is added in reaction 2 hours, and stirring decoloration 0.6 hour is filtered while hot, and filtrate first naturally cools to 20 ~ 30 DEG C, then
At 0 ~ 5 DEG C, keep the temperature 2.5 hours, filtering, washed with a small amount of dehydrated alcohol it is colourless to cleaning solution, 55 ~ 60 DEG C be dried in vacuo
3.5 hours, obtain Sulfamonomethoxime Sodium 20.42g, yield 94.67%.Sulfamonomethoxime Sodium is white crystalline powder
End, purity 99.4%.Waste liquid weakly acidic pH is filtered during the preparation process.
Embodiment 8
A kind of preparation method of Sulfamonomethoxime Sodium, comprising the following steps:
By 20g daimeton, 3.0g sodium hydroxide is added in 300ml ethyl alcohol, under the conditions of 70 ~ 82 DEG C of temperature, stirring
0.9g active carbon is added in reaction 1.5 hours, and stirring decoloration 0.5 hour is filtered while hot, and filtrate first naturally cools to 20 ~ 30 DEG C,
Again at 0 ~ 5 DEG C, keep the temperature 1.5 hours, filtering, washed with a small amount of dehydrated alcohol it is colourless to cleaning solution, 55 ~ 60 DEG C be dried in vacuo
2 hours, obtain Sulfamonomethoxime Sodium 20.75g, yield 96.20%.Sulfamonomethoxime Sodium is white crystalline powder,
Purity is 99.3%.Waste liquid weakly acidic pH is filtered during the preparation process.
Embodiment 9
A kind of preparation method of Sulfamonomethoxime Sodium, comprising the following steps:
By 20g daimeton, 3.0g sodium hydroxide is added in 250ml ethyl alcohol, under the conditions of 70 ~ 82 DEG C of temperature, stirring
0.75g active carbon is added in reaction 0.5 hour, and stirring decoloration 0.8 hour is filtered while hot, and filtrate first naturally cools to 20 ~ 30 DEG C,
Again at 0 ~ 5 DEG C, keep the temperature 1 hour, filtering, washed with a small amount of dehydrated alcohol it is colourless to cleaning solution, 55 ~ 60 DEG C be dried in vacuo 4
Hour, obtain Sulfamonomethoxime Sodium 20.70g, yield 95.97%.Sulfamonomethoxime Sodium is white crystalline powder,
Purity is 99.3%.Waste liquid weakly acidic pH is filtered during the preparation process.
Embodiment 10
A kind of preparation method of Sulfamonomethoxime Sodium, comprising the following steps:
By 20g daimeton, 2.8g sodium hydroxide is added in 250ml ethyl alcohol, under the conditions of 70 ~ 82 DEG C of temperature, stirring
0.75g active carbon is added in reaction 1.5 hours, and stirring decoloration 0.3 hour is filtered while hot, and filtrate first naturally cools to 20 ~ 30 DEG C,
Again at 0 ~ 5 DEG C, keep the temperature 3 hours, filtering, washed with a small amount of dehydrated alcohol it is colourless to cleaning solution, 55 ~ 60 DEG C be dried in vacuo 3
Hour, obtain Sulfamonomethoxime Sodium 20.90g, yield 96.89%.Sulfamonomethoxime Sodium is white crystalline powder,
Purity is 99.3%.Waste liquid weakly acidic pH is filtered during the preparation process.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those skilled in the art,
Without depart from that overall concept of the invention, several changes and improvements can also be made, these also should be considered as of the invention
Protection scope.
Claims (8)
1. a kind of preparation method of Sulfamonomethoxime Sodium, it is characterised in that: the following steps are included:
(1) daimeton, sodium hydroxide are added in organic solvent, under the conditions of 54 ~ 98 DEG C of temperature, are stirred to react
0.5-2 hours, obtain solution A；
(2) active carbon is added to solution A, stirring decoloration 0.3-0.8 hours filters while hot, obtains filtrate；
(3) filtrate first naturally cools to 20 ~ 30 DEG C, then at 0 ~ 5 DEG C, keeps the temperature 1-3 hours, and filtering obtains filter residue；
(4) wash filter residue with a small amount of dehydrated alcohol, 55 ~ 60 DEG C vacuum drying 2-4 hours, obtain Sulfamonomethoxime Sodium.
2. the preparation method of Sulfamonomethoxime Sodium according to claim 1, it is characterised in that: in the step (1),
The mass ratio of daimeton and sodium hydroxide is 1:(0.13 ~ 0.15).
3. the preparation method of Sulfamonomethoxime Sodium according to claim 2, it is characterised in that: in the step (1),
The mass ratio of daimeton and sodium hydroxide is 1:0.14.
4. the preparation method of Sulfamonomethoxime Sodium according to claim 1, it is characterised in that: in the step (1),
The mass volume ratio of daimeton and organic solvent is 1:(8.5 ~ 15), unit g/ml.
5. the preparation method of Sulfamonomethoxime Sodium according to claim 4, it is characterised in that: in the step (1),
The mass volume ratio of daimeton and organic solvent is 1:10, unit g/ml.
6. the preparation method of Sulfamonomethoxime Sodium according to claim 1, it is characterised in that: in the step (1),
Used organic solvent is ethyl alcohol.
7. the preparation method of Sulfamonomethoxime Sodium according to claim 1, it is characterised in that: in the step (2),
Active carbon and the volume mass of organic solution ratio are 0.3:100, unit g/ml.
8. according to claim 1 between the sulfanilamide (SN) of the preparation method preparation of Sulfamonomethoxime Sodium described in -7 any claims
Sulfamonomethoxine sodium.
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|---|---|---|---|
| CN201710464902.4A CN109134387A (en) | 2017-06-19 | 2017-06-19 | A kind of preparation method of Sulfamonomethoxime Sodium and Sulfamonomethoxime Sodium prepared by this method |
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| CN201710464902.4A CN109134387A (en) | 2017-06-19 | 2017-06-19 | A kind of preparation method of Sulfamonomethoxime Sodium and Sulfamonomethoxime Sodium prepared by this method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111471022A (en) * | 2020-03-20 | 2020-07-31 | 瑞普（天津）生物药业有限公司 | Sulfamonomethoxine sodium crystal form and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1082031A (en) * | 1993-05-20 | 1994-02-16 | 郑州市孝义制药厂 | The preparation method of sulfamonomethoxine |
| WO2011012722A1 (en) * | 2009-07-31 | 2011-02-03 | Ascendis Pharma As | Prodrugs containing an aromatic amine connected by an amido bond to a linker |
| CN103319418A (en) * | 2013-06-19 | 2013-09-25 | 扬州天和药业有限公司 | Method for preparing sulfamonomethoxine sodium |
| CN105294577A (en) * | 2015-11-23 | 2016-02-03 | 和夏化学(太仓)有限公司 | Preparation method for sulfanilamide-6-methoxypyrimidine |
| CN106565616A (en) * | 2016-11-14 | 2017-04-19 | 杭州洪晟生物技术股份有限公司 | Preparation method of antibacterial veterinary drug sulfamonomethoxine sodium |
-
2017
- 2017-06-19 CN CN201710464902.4A patent/CN109134387A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1082031A (en) * | 1993-05-20 | 1994-02-16 | 郑州市孝义制药厂 | The preparation method of sulfamonomethoxine |
| WO2011012722A1 (en) * | 2009-07-31 | 2011-02-03 | Ascendis Pharma As | Prodrugs containing an aromatic amine connected by an amido bond to a linker |
| CN103319418A (en) * | 2013-06-19 | 2013-09-25 | 扬州天和药业有限公司 | Method for preparing sulfamonomethoxine sodium |
| CN105294577A (en) * | 2015-11-23 | 2016-02-03 | 和夏化学(太仓)有限公司 | Preparation method for sulfanilamide-6-methoxypyrimidine |
| CN106565616A (en) * | 2016-11-14 | 2017-04-19 | 杭州洪晟生物技术股份有限公司 | Preparation method of antibacterial veterinary drug sulfamonomethoxine sodium |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111471022A (en) * | 2020-03-20 | 2020-07-31 | 瑞普（天津）生物药业有限公司 | Sulfamonomethoxine sodium crystal form and preparation method thereof |
| CN111471022B (en) * | 2020-03-20 | 2024-05-14 | 瑞普（天津）生物药业有限公司 | Sulfamethoxypyrimidine sodium crystal form and preparation method thereof |
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