CN109400581A - A method of improving nicosulfuron content - Google Patents
A method of improving nicosulfuron content Download PDFInfo
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- CN109400581A CN109400581A CN201810826082.3A CN201810826082A CN109400581A CN 109400581 A CN109400581 A CN 109400581A CN 201810826082 A CN201810826082 A CN 201810826082A CN 109400581 A CN109400581 A CN 109400581A
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- phonetic
- nicosulfuron
- cigarette
- toluene
- content
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D401/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
- C07D401/02—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
- C07D401/12—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings linked by a chain containing hetero atoms as chain links
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Plural Heterocyclic Compounds (AREA)
Abstract
The present invention provides a kind of methods for improving nicosulfuron content, method includes the following steps, the phonetic raw medicine of cigarette is added at 30-90 DEG C to toluene and stirs 30min, it is cooled to 40 DEG C of suction filtrations, pure nicosulfuron can be obtained in drying filter cake, the present invention provides the content that high method can effectively improve nicosulfuron in the phonetic raw medicine of cigarette, enhances the competitiveness of product in market；Save labor cost；High income, the three wastes are few compared with other methods, low energy consumption, are suitable for industrially promoting the use of.
Description
Technical field
The present invention relates to drug purification technique fields, and in particular to a method of improve nicosulfuron content.
Background technique
Nicosulfuron is Japanese Ishihara Sangyo Kaisha, Ltd.'s discovery, and late 1980s combine with DuPont Corporation
The sulfonylurea systemic herbicide of exploitation.
High-content nicosulfuron raw medicine is relatively fewer in the market, and especially 97% or more cigarette is phonetic, and supply falls short of demand, due to closing
Relatively long at the process flow of nicosulfuron, in addition the country synthesizes, the phonetic process route of cigarette is not advanced enough, and content and yield are all
It is relatively low, and since solubility of the common organic solvent to nicosulfuron is all smaller, it is difficult the side by recrystallization
Formula improves the content of nicosulfuron.And the method for recrystallization is generally required by complexity such as heating, heat preservation, cooling, filterings
Operating process.Again since during raw medicine synthesizes, in order to improve the yield of product most possibly, our feed intake is matched
Than often a raw material being used to react another raw material completely, excessive raw materials recovery is applied.Nicosulfuron synthesizes
It allows intermediate amine ester total overall reaction, improves the proportion of another main reaction object pyrilamine, that is, pyrilamine is excessive, and by pyrimidine
Amine recovery.But pyrilamine is soluble in the toluene of heat and solubility is small in cold toluene, that is, the solubility of pyrilamine
Variation with temperature is obvious, and therefore, during product is isolated in last cooling, excessive pyrilamine is also easy analysis
Out, pyrilamine has just easily been brought into our product in this way.Therefore the pyrilamine brought into product is reduced, or removes band in product
The pyrilamine entered opposite can improve content.Test prove be added at a certain temperature a certain amount of toluene can dissolve it is certain
Pyrilamine, is added that toluene is excessive or temperature crosses that high product loss is more, and yield reduces, and is added that toluene is less or temperature is too low, phonetic
Pyridine amine is taken away less, and product content cannot improve.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of method for improving nicosulfuron content, the method packets
Following steps are included, the phonetic raw medicine of cigarette is added at 30-90 DEG C to toluene and stirs 30min, is cooled to 40 DEG C of suction filtration, drying filter cake is
Pure nicosulfuron can be obtained.
Preferably, above-mentioned toluene and the phonetic raw medicine mass ratio of cigarette are 3-10:20.
Preferably, above-mentioned toluene and the phonetic raw medicine mass ratio of cigarette are 8:20.
Preferably, above-mentioned toluene and the phonetic raw medicine mass ratio of cigarette are 9:20.
Preferably, the phonetic raw medicine of cigarette is added at 70 DEG C in the above method.
The invention has the benefit that
(1) method provided by the invention can effectively improve the content of nicosulfuron in the phonetic raw medicine of cigarette, enhance the product
The market competitiveness.
(2) method provided by the invention is simple and easy to get compared with other methods, saves labor cost.
(3) high income, the three wastes are few compared with other methods, low energy consumption for method provided by the invention, are suitable for industrially pushing away
It is wide to use.
Detailed description of the invention
Fig. 1 is the product analysis map that directly cooling filters drying；
Fig. 2 is plus toluene stirs after being warming up to 70 DEG C of heat preservation 30min, and cooling filters the analysis map of products obtained therefrom.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with implementation of the invention
Example, technical scheme in the embodiment of the invention is clearly and completely described.Based on the embodiments of the present invention, this field
Those of ordinary skill's every other embodiment obtained without creative efforts, belongs to protection of the present invention
Range.
Embodiment 1:
It takes the phonetic product synthesis insulation reaction of cigarette to terminate material, is cooled to 40 degree and filters to obtain filter cake, 400g filter cake is taken to be divided into two
Equal portions, it is a directly to dry；Portion is added toluene and is warming up to 70 degree, stirs 30 minutes, then the drying of the 40 degree of suction filtrations that cool down, filter cake,
As a result as shown in Fig. 1 and Fig. 2 in table 1, Figure of description.
Embodiment 2:
It takes the phonetic product synthesis insulation reaction of cigarette to terminate material, is cooled to 40 degree and filters to obtain filter cake, be divided into several equal portions, every part adds
The toluene for entering isodose is warming up to different temperatures, stirs 30 minutes, 40 degree filter, filter cake drying, comparison products obtained therefrom content and
Yield.The results are shown in Table 1.
Embodiment 3:
Take with batch phonetic centrifugation wet product of cigarette, be added weight not equal toluene 70 DEG C stirrings heat preservation 30 minutes it is subsequent cool down from
The heart, the results are shown in Table 3.
Table 1
Table 2
Table 3
It can be obtained from Fig. 1 and Fig. 2: add toluene to wash the peak that rear 3.2min goes out and drop to 1.8% by original 3.5%, product peak
It is 97.0% that area is risen to by original 94.4%, and it is 95.7% that content, which is also risen to by original 94.1,.In conjunction in table 1 twice
The experiment gained phonetic dry product quality of cigarette can greatly improve the phonetic sulphur of cigarette in the phonetic raw medicine of cigarette it can be concluded that toluene is added at a certain temperature
Grand content, and do not influence yield；As can be drawn from Table 2, after toluene being added, 70 degree of insulating product contents and percentage amount are all most
It is good, that is, plus toluene 70 degree of heat preservations washing can improve content and not influence product yield；200g cigarette as can be drawn from Table 3
The washing of 80g, 90g toluene is added in phonetic wet product, and products obtained therefrom content and yield are best.
Can be obtained by the three groups of above tests: toluene washing is added at 70 DEG C for the phonetic raw medicine of cigarette can significantly improve the phonetic sulphur of cigarette
Grand content and yield is not reduced, the optimum proportioning of toluene is added are as follows: the phonetic wet product percentage amount of cigarette: toluene by weight=1.6-2.0:1.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (5)
1. a kind of method for improving nicosulfuron content, which is characterized in that the described method comprises the following steps, the phonetic raw medicine of cigarette is existed
Toluene is added at 30-90 DEG C and stirs 30min, is cooled to 40 DEG C of suction filtrations, pure nicosulfuron can be obtained in drying filter cake.
2. the method according to claim 1 for improving nicosulfuron content, which is characterized in that the toluene and the phonetic raw medicine of cigarette
Mass ratio is 3-10:20.
3. the method according to claim 2 for improving nicosulfuron content, which is characterized in that the toluene and the phonetic raw medicine of cigarette
Mass ratio is 8:20.
4. the method according to claim 2 for improving nicosulfuron content, which is characterized in that the toluene and the phonetic raw medicine of cigarette
Mass ratio is 9:20.
5. the method according to claim 1 for improving nicosulfuron content, which is characterized in that by the phonetic original of cigarette in the method
Medicine is added at 70 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810826082.3A CN109400581A (en) | 2018-09-20 | 2018-09-20 | A method of improving nicosulfuron content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810826082.3A CN109400581A (en) | 2018-09-20 | 2018-09-20 | A method of improving nicosulfuron content |
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| CN109400581A true CN109400581A (en) | 2019-03-01 |
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| CN201810826082.3A Pending CN109400581A (en) | 2018-09-20 | 2018-09-20 | A method of improving nicosulfuron content |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111793059A (en) * | 2020-07-20 | 2020-10-20 | 安徽华星化工有限公司 | Refining method for obtaining high-content nicosulfuron by acid-base precipitation decoloring treatment |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503403A (en) * | 2009-03-10 | 2009-08-12 | 天津市农药研究所 | Preparation of sulfonylurea herbicide nicosulfuron |
| CN102382049A (en) * | 2011-12-20 | 2012-03-21 | 安徽丰乐农化有限责任公司 | Method for synthesizing 2-ethoxycarbonylaminosulfonyl-N,N-dimethyl nicotinamide |
| WO2016014814A1 (en) * | 2014-07-25 | 2016-01-28 | E. I. Du Pont De Nemours And Company | Pyridones as herbicides |
| CN106749183A (en) * | 2016-11-12 | 2017-05-31 | 江苏长青生物科技有限公司 | The synthesis technique of nicosulfuron active compound |
-
2018
- 2018-09-20 CN CN201810826082.3A patent/CN109400581A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503403A (en) * | 2009-03-10 | 2009-08-12 | 天津市农药研究所 | Preparation of sulfonylurea herbicide nicosulfuron |
| CN102382049A (en) * | 2011-12-20 | 2012-03-21 | 安徽丰乐农化有限责任公司 | Method for synthesizing 2-ethoxycarbonylaminosulfonyl-N,N-dimethyl nicotinamide |
| WO2016014814A1 (en) * | 2014-07-25 | 2016-01-28 | E. I. Du Pont De Nemours And Company | Pyridones as herbicides |
| CN106749183A (en) * | 2016-11-12 | 2017-05-31 | 江苏长青生物科技有限公司 | The synthesis technique of nicosulfuron active compound |
Non-Patent Citations (1)
| Title |
|---|
| 贾淑敏: "《嘧啶磺酰脲除草剂的纯化与分析》", 《中国优秀硕士学位论文全文数据库（电子期刊）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111793059A (en) * | 2020-07-20 | 2020-10-20 | 安徽华星化工有限公司 | Refining method for obtaining high-content nicosulfuron by acid-base precipitation decoloring treatment |
| CN111793059B (en) * | 2020-07-20 | 2021-06-25 | 安徽华星化工有限公司 | Refining method for obtaining high-content nicosulfuron by acid-base precipitation decoloring treatment |
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