CN108569980A - The method of purification of impurity in a kind of iprovalicarb active compound - Google Patents
The method of purification of impurity in a kind of iprovalicarb active compound Download PDFInfo
- Publication number
- CN108569980A CN108569980A CN201810636797.2A CN201810636797A CN108569980A CN 108569980 A CN108569980 A CN 108569980A CN 201810636797 A CN201810636797 A CN 201810636797A CN 108569980 A CN108569980 A CN 108569980A
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- CN
- China
- Prior art keywords
- impurity
- iprovalicarb
- active compound
- purification
- filtrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
Abstract
The invention discloses a kind of methods of purification of impurity in iprovalicarb active compound, include the following steps：1) it is dissolved by heating after being mixed with a certain amount of methanol as raw material using iprovalicarb crude product；2) wait for that solution cooled and filtered takes first-time filtrate；3) first-time filtrate is gradually dropped after solid is precipitated in water, filters to take secondary filtrate；4) it is eluant, eluent secondary filtrate decompression to be evaporated off after solvent with ethyl acetate and petroleum ether, it is carried out removing solvent under reduced pressure after separation obtains target impurity solution with column chromatography silica gel, obtains 3 methyl N of target impurity 2 (isopropoxyamino) (1 p tolylethyl) butanamide.Easy to operate, low manufacture cost of the invention, can get sample of the purity 90% or more.
Description
Technical field
The present invention relates to fungicide technical field, more particularly to the method for purification of impurity in a kind of iprovalicarb active compound.
Background technology
Iprovalicarb be amino-acid ester analog derivative, be one kind aim at prevention downy mildew and specifically developed wide-spectrum bactericide,
Its lasting period is long, especially good to the downy mildew preventive effect on the crops such as cucumber, grape.
According to China's laws and regulations requirement, pesticide must carry out registration experiment, and pesticide original medicine must then carry out full proximate analysis
Experiment needs the impurity to content higher than 0.1% to carry out qualitative and quantitative analysis, during this measurement analysis, it is necessary to
It to be compareed using standard substance to provide structure and content, is essential.
2- (isopropoxyamino) -3-methyl-N- (1-p-tolylethyl) butanamide is iprovalicarb active compound
In process of production, the impurity isopropanol contained in iprovalicarb raw materials for production isopropyl chloroformate and valine and 1- (4- first
Phenyl) ethamine reaction generate impurity, content of the impurity in iprovalicarb active compound be usually above 0.1%, need use standard
Substance carries out qualitative and quantitative analysis to it.But there has been no No. CAS at present for the substance, also standard items not on sale on the market
It is commercially available.
Invention content
In view of the deficiencies of the prior art, the technical problem to be solved is that provide a kind of convenient, of low cost, ring by the present invention
The method of purification of impurity in the iprovalicarb active compound of guarantor, so as to the substance of quick obtaining to high-purity, and then for examining detection.
The present invention is so that above-mentioned technical problem is addressed by the following technical programs.
The method of purification of impurity, includes the following steps in a kind of iprovalicarb active compound：1) using iprovalicarb crude product as raw material and one
It is dissolved by heating after quantitative methanol mixing；2) wait for that solution cooled and filtered takes first-time filtrate；3) first-time filtrate is gradually dropped in water
After solid is precipitated, secondary filtrate is filtered to take；4) it is elution secondary filtrate decompression to be evaporated off after solvent with ethyl acetate and petroleum ether
Agent is carried out removing solvent under reduced pressure after separation obtains target impurity solution with column chromatography silica gel, obtains target impurity
2-(isopropoxyamino)-3-methyl-N-(1-p-tolylethyl)butanamide。
Preferably, the volume proportion of ethyl acetate and petroleum ether is 1 in eluant, eluent:10~1:20.
Preferably, target impurity purity is more than 90%.
Beneficial effects of the present invention：Easy to operate, low manufacture cost of the invention, can get
2- (isopropoxyamino) -3-methyl-N- (1-p-tolylethyl) butanamide purity 90% with
On sample.
Specific implementation mode
In order to facilitate the present invention is understood, the preferred embodiment of invention now given below is detailed to present invention progress to retouch
It states.
Embodiment 1
About 53g iprovalicarb crude products are added in 250mL beakers, about 160mL methanol is added, heating is allowed to be dissolved to clarification,
It waits for that solution is cooled to room temperature, filters the solution and take first-time filtrate, first-time filtrate is gradually dropped in 400mL water, solid is precipitated, mistake
It is eluant, eluent that the secondary filtrate decompression of leaching, which is evaporated off after solvent with ethyl acetate and petroleum ether, is detached, is washed with column chromatography silica gel
Ethyl acetate in de- agent：Petroleum ether is 1：20 (v/v) remove solvent under reduced pressure after obtaining target impurity solution, obtain purity and exist
90% or more target impurity
2-(isopropoxyamino)-3-methyl-N-(1-p-tolylethyl)butanamide。
Claims (3)
1. the method for purification of impurity in a kind of iprovalicarb active compound, it is characterized in that：Include the following steps：1) it is original with iprovalicarb crude product
Material dissolves by heating after being mixed with a certain amount of methanol；2) wait for that solution cooled and filtered takes first-time filtrate；3) first-time filtrate is gradually dripped
Enter after solid is precipitated in water, filters to take secondary filtrate；4) ethyl acetate and petroleum ether are used after solvent being evaporated off in secondary filtrate decompression
For eluant, eluent, is carried out removing solvent under reduced pressure after separation obtains target impurity solution with column chromatography silica gel, obtain target impurity 2-
(isopropoxyamino)-3-methyl-N-(1-p-tolylethyl)butanamide。
2. the method for purification of impurity in iprovalicarb active compound according to claim 1, it is characterized in that：Ethyl acetate in eluant, eluent
Volume proportion with petroleum ether is 1:10~1:20.
3. the method for purification of impurity in iprovalicarb active compound according to claim 1, it is characterized in that：Target impurity purity is more than
90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810636797.2A CN108569980A (en) | 2018-06-20 | 2018-06-20 | The method of purification of impurity in a kind of iprovalicarb active compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810636797.2A CN108569980A (en) | 2018-06-20 | 2018-06-20 | The method of purification of impurity in a kind of iprovalicarb active compound |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108569980A true CN108569980A (en) | 2018-09-25 |
Family
ID=63573384
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810636797.2A Pending CN108569980A (en) | 2018-06-20 | 2018-06-20 | The method of purification of impurity in a kind of iprovalicarb active compound |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108569980A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5453531A (en) * | 1990-08-25 | 1995-09-26 | Bayer Aktiengesellschaft | Substituted valinamide derivatives |
| CN1098250C (en) * | 1996-08-02 | 2003-01-08 | 拜尔公司 | Process for preparing substituted valine amide derivatives |
| CN1193020C (en) * | 2000-04-03 | 2005-03-16 | 伊哈拉化学工业株式会社 | Process for preparing amic acid esters |
-
2018
- 2018-06-20 CN CN201810636797.2A patent/CN108569980A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5453531A (en) * | 1990-08-25 | 1995-09-26 | Bayer Aktiengesellschaft | Substituted valinamide derivatives |
| CN1098250C (en) * | 1996-08-02 | 2003-01-08 | 拜尔公司 | Process for preparing substituted valine amide derivatives |
| CN1193020C (en) * | 2000-04-03 | 2005-03-16 | 伊哈拉化学工业株式会社 | Process for preparing amic acid esters |
Non-Patent Citations (2)
| Title |
|---|
| MAN SUN等: "Design, synthesis, and fungicidal activities of imino diacid analogs of valine amide fungicides", 《BIOORGANIC & MEDICINAL CHEMISTRY LETTERS》 * |
| 卢平，张钰萍: "杀菌剂异丙菌胺原药的反相高效液相色谱分析方法", 《农药科学与管理》 * |
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|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180925 |
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| WD01 | Invention patent application deemed withdrawn after publication |