CN111423346B - Preparation method of clethodim lithium salt standard sample - Google Patents
Preparation method of clethodim lithium salt standard sample Download PDFInfo
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- CN111423346B CN111423346B CN202010434138.8A CN202010434138A CN111423346B CN 111423346 B CN111423346 B CN 111423346B CN 202010434138 A CN202010434138 A CN 202010434138A CN 111423346 B CN111423346 B CN 111423346B
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- clethodim
- acetone
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- lithium salt
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/14—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides
- C07C319/20—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides by reactions not involving the formation of sulfide groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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- Organic Chemistry (AREA)
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Abstract
The invention relates to a preparation method of clethodim lithium salt standard sample, which comprises the following steps: (1) adding clethodim and anhydrous lithium hydroxide into acetone by taking acetone as a solvent, wherein the mass ratio of clethodim to lithium hydroxide is 1.1-1.3: 1; (2) stirring and heating to 30-60 ℃, and reacting for 8-12 hours; (3) naturally cooling to 10-15 ℃, separating out crystals, filtering to obtain crystals, and washing with acetone; (4) and drying the crystals in vacuum, crushing and sieving to obtain the final standard sample. The method is simple and easy to operate, and the prepared standard sample has high content and good stability and is not easy to agglomerate.
Description
Technical Field
The invention relates to the technical field of chemical preparation, and particularly relates to a preparation method of a clethodim lithium salt standard sample.
Background
The clethodim lithium salt is a standard sample for quantitative analysis of clethodim technical materials, and the clethodim lithium salt obtained by the conventional synthesis method at present has the defects of low content, short storage time, poor stability, easiness in caking and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the preparation method of the clethodim lithium salt standard sample, which is simple and easy to operate, and the prepared standard sample has high purity and good stability.
The invention is realized by the following technical scheme:
the preparation method of the clethodim lithium salt standard sample comprises the following steps:
(1) adding clethodim and anhydrous lithium hydroxide into acetone by taking acetone as a solvent, wherein the mass ratio of clethodim to lithium hydroxide is 1.1-1.3: 1;
(2) stirring and heating to 30-60 ℃, and reacting for 8-12 hours;
(3) naturally cooling to 10-15 ℃, separating out crystals, filtering to obtain crystals, and washing with acetone;
(4) and drying the crystals in vacuum, crushing and sieving to obtain the final standard sample.
Further, in the step (4), the drying temperature is 30 ℃ to 50 ℃, and the vacuum degree is-0.08 MPa to-0.09 MPa.
Further, acetone is analytically pure 99% content acetone.
The invention has the beneficial effects that:
the synthesis conditions of the clethodim lithium salt are improved and adjusted, so that the content yield of the clethodim lithium salt is increased, the stability is improved, the storage time is prolonged, and the product is not easy to agglomerate and is easy to crush.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present solution is explained below by way of specific embodiments.
A preparation method of clethodim lithium salt standard samples comprises the following steps:
(1) acetone is used as a solvent, the acetone is used as acetone with the content of 99% of analytical purity, clethodim and anhydrous lithium hydroxide are added into the acetone, and the mass ratio of the clethodim to the lithium hydroxide is 1.1-1.3: 1;
(2) stirring and heating to 30-60 ℃, and reacting for 8-12 hours;
(3) naturally cooling to 10-15 ℃, separating out crystals, filtering to obtain crystals, and washing with acetone;
(4) and drying the crystals in vacuum, crushing and sieving to obtain the final standard sample.
Further, in the step (4), the drying temperature is 30 ℃ to 50 ℃, and the vacuum degree is-0.08 MPa to-0.09 MPa.
Example 1:
44.94g of clethodim raw drug with the mass fraction of 88%, 300ml of acetone with the content of 99% of analytical purity and 2.41g of anhydrous lithium hydroxide are put into a 500ml dry four-neck flask, stirred, heated to 30 ℃, stirred for 12 hours, naturally cooled to 10 ℃, crystallized, filtered, washed by 30ml of acetone for 3 times, put into a vacuum oven for drying at 30 ℃, weighed 35.06g, the content is 99.0%, and the yield is 95%.
Compared with the existing products, the content of the existing products is reduced and the existing products are caked after being stored for one month, and the products prepared by the method can be stored for half a year without changing the content and are not easy to block.
Example 2:
in a 500ml dry four-neck flask, 50.80g of 92% clethodim technical, 300ml of acetone with 99% of analytical purity and 2.41g of anhydrous lithium hydroxide are added, stirred, heated to 60 ℃, stirred for 8 hours, naturally cooled to 10 ℃, crystallized, filtered, filter cake is washed by 30ml of acetone for 3 times, and the filter cake is put into a vacuum oven for drying at 50 ℃, 36.17g is weighed, the content is 99.0%, and the yield is 98%.
Compared with the existing products, the content of the existing products is reduced and the existing products are caked after being stored for one month, and the products prepared by the method can be stored for half a year without changing the content and are not easy to block.
Comparative example:
in a 500ml dry four-neck flask, 50.80g of 92% clethodim technical, 300ml of acetone with 99% of analytical purity and 2.41g of lithium hydroxide are added, stirred, heated to 60 ℃, stirred for 8 hours, naturally cooled to 10 ℃, precipitated and crystallized, filtered, a filter cake is washed by 30ml of acetone for 3 times, put into a vacuum oven for drying at 50 ℃, weighed 32.48g, with 90.0% of content and 80% of yield.
Compared with the comparative examples in the embodiment 1 and the embodiment 2, the preparation method provided by the invention has the advantages that the standard sample content of the clethodim lithium salt is high, and the yield is high.
Of course, the above description is not limited to the above examples, and the undescribed technical features of the present invention can be implemented by or using the prior art, and will not be described herein again; the above embodiments are merely for illustrating the technical solutions of the present invention and not for limiting the present invention, and the present invention has been described in detail with reference to the preferred embodiments, and those skilled in the art should understand that changes, modifications, additions or substitutions which are made by those skilled in the art within the spirit of the present invention are also within the scope of the claims of the present invention.
Claims (3)
1. A preparation method of clethodim lithium salt standard samples is characterized by comprising the following steps: the method comprises the following steps:
(1) adding clethodim and anhydrous lithium hydroxide into acetone by taking acetone as a solvent, wherein the mass ratio of clethodim to lithium hydroxide is 1.1-1.3: 1;
(2) stirring and heating to 30-60 ℃, and reacting for 8-12 hours;
(3) naturally cooling to 10-15 ℃, separating out crystals, filtering to obtain crystals, and washing with acetone;
(4) and drying the crystals in vacuum, crushing and sieving to obtain the final standard sample.
2. The process for preparing a clethodim lithium salt standard according to claim 1, wherein: in the step (4), the drying temperature is 30 ℃ to 50 ℃, and the vacuum degree is-0.08 MPa to-0.09 MPa.
3. The process for preparing a clethodim lithium salt standard according to claim 1, wherein: acetone is analytically pure 99% content acetone.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010434138.8A CN111423346B (en) | 2020-05-21 | 2020-05-21 | Preparation method of clethodim lithium salt standard sample |
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| CN202010434138.8A CN111423346B (en) | 2020-05-21 | 2020-05-21 | Preparation method of clethodim lithium salt standard sample |
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| CN111423346A CN111423346A (en) | 2020-07-17 |
| CN111423346B true CN111423346B (en) | 2022-05-03 |
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| CN116283685A (en) * | 2022-12-21 | 2023-06-23 | 宁夏格瑞精细化工有限公司 | Synthesis method of clethodim lithium salt standard sample |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85107306A (en) * | 1984-06-11 | 1987-04-15 | 切夫尔昂研究公司 | 2-[1-(3-chloroallyloxyamino amino) alkyl fork]-5-alkyl-thio-alkyl-hexanaphthene-1,3-diketone herbicide |
| JPS6289653A (en) * | 1985-09-30 | 1987-04-24 | Nippon Soda Co Ltd | Cyclohexanedione derivative |
| US4741768A (en) * | 1985-11-15 | 1988-05-03 | Chevron Research Company | Herbicidal substituted 2-[1-(3-trans-chloro-allyloxyamino)alkylidene]-cyclohexane dione salts |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10045131A1 (en) * | 2000-09-13 | 2002-03-21 | Basf Ag | Process for the preparation of a cyclohexenone oxime ether lithium salt, products obtainable therewith, their use and corresponding crop protection agents |
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2020
- 2020-05-21 CN CN202010434138.8A patent/CN111423346B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85107306A (en) * | 1984-06-11 | 1987-04-15 | 切夫尔昂研究公司 | 2-[1-(3-chloroallyloxyamino amino) alkyl fork]-5-alkyl-thio-alkyl-hexanaphthene-1,3-diketone herbicide |
| JPS6289653A (en) * | 1985-09-30 | 1987-04-24 | Nippon Soda Co Ltd | Cyclohexanedione derivative |
| US4741768A (en) * | 1985-11-15 | 1988-05-03 | Chevron Research Company | Herbicidal substituted 2-[1-(3-trans-chloro-allyloxyamino)alkylidene]-cyclohexane dione salts |
Non-Patent Citations (1)
| Title |
|---|
| 环己烯酮类除草剂——烯草酮的合成;孙光强 等;《现代农药》;20110228;第24-26页 * |
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