CN102442958A - Preparation method of isomer-removed tebuconazole - Google Patents
Preparation method of isomer-removed tebuconazole Download PDFInfo
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- CN102442958A CN102442958A CN2010105174891A CN201010517489A CN102442958A CN 102442958 A CN102442958 A CN 102442958A CN 2010105174891 A CN2010105174891 A CN 2010105174891A CN 201010517489 A CN201010517489 A CN 201010517489A CN 102442958 A CN102442958 A CN 102442958A
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- isomer
- tebuconazole
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- weakly alkaline
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Abstract
The invention discloses a preparation method of isomer-removed tebuconazole. In the preparation method, firstly, tebuconazole, a tebuconazole isomer mixed solvent, mixed impurities, the oilness and residue at a kettle from which a crystal cannot be separated are treated. The preparation method comprises the following steps of: firstly, adding acid in the reside at the kettle to enable the reside at the kettle to form salt; secondly, feeding water containing soda in the salt and hydrolyzing; after hydrolyzing, adding a solvent and reefing; and finally, drying the obtained material and then measuring the content of the isomer to be extremely high. The preparation method is characterized in that alkalescent salt substances are added in the tebuconazole containing the isomer; the temperature is raised to be 120DEG C and then the temperature is kept for 1-5 hours; and the isomer is converted into the tebuconazole. The preparation method disclosed by the invention has the advantages that the alkalescent salt substances are adopted so as to effectively reduce the inverse transformation of the reaction and increase the yield.
Description
Technical field
The present invention relates to a kind of tebuconazole and remove the preparation method of isomer, specifically is the preparation method that a kind of tebuconazole that can prevent effectively that reversed reaction from producing is removed isomer.
Background technology
The tebuconazole structural formula:
In synthetic tebuconazole, can generate a kind of isomer,
The isomer structure formula:
Concerning farm crop, existing of isomer is nonsensical, and it has consumed starting material, has influenced the content of tebuconazole, therefore will isomer be removed.
In the original process, the conversion of isomer generally adds caustic soda, and when adding the caustic soda conversion, general speed of response is too fast, control not too easily, and alkalescence is too strong, and tebuconazole can produce reversed reaction.
Summary of the invention
Main task of the present invention is to provide a kind of tebuconazole to remove the preparation method of isomer, at first to tebuconazole, and tebuconazole isomer mixed solvent, impurity blended; Oiliness, crystal analyse that the still that does not come out is residual to be handled, and step is following: in still is residual, add sour earlier; Make the residual salify of still, in salt, drop into the buck hydrolysis then, after hydrolysis is accomplished; Add solvent treatment, behind the drying materials that obtains, the content that records isomer is bigger than normal; It is characterized in that: in the above-mentioned tebuconazole that contains isomer, add the weakly alkaline salts substances, be warming up to 120 back insulations 1-5 hour, isomer is converted into tebuconazole.
Further, the structural formula of said isomer is:
Further, said weakly alkaline salts substances is a potassium class weakly alkaline salt.
Further, said weakly alkaline salts substances: the mol ratio that contains the tebuconazole of isomer is 1: 4.
The invention has the advantages that: adopt the weakly alkaline salts substances, effectively reduce the reverseization of reaction, improve yield.
Embodiment
The comparative example 1
Former technology:
Tebuconazole 93% (isomer 3%): 60g, sodium hydroxide: 5 grams, be warmed up to 120 ℃ of holding-zones, be incubated sampling in 1 hour, the tebuconazole 94.2% of survey, isomer 0.2%, epoxy 2.6%; Purify with 150 gram ethers and ethyl acetate class mixed solvent then, oven dry gets material 48.1 grams, and content is 97.1%.
Technology of the present invention:
Tebuconazole 93% (isomer 3%): 60g, saleratus: 5 grams, heat up 120 ℃, be incubated sampling in 1 hour, the tebuconazole 95.5% of survey, isomer 0.2%, epoxy 0.55%; With 150 grams, ethers and ethyl acetate class mixed solvent are purified then, and oven dry gets material 50 grams, and content is 97.2%.
The comparative example 2
Former technology:
Tebuconazole 93% (isomer 3%): 60g, caustic soda: 5 grams, be warmed up to 120 ℃ of holding-zones, be incubated sampling in 3 hours, tebuconazole is 90.5%, and isomer is 0.05%, and epoxy is 6.0%; With 150 grams, ethers and ethyl acetate class mixed solvent are purified then, and oven dry gets material 45.2 grams, content is 96.9%.
Technology of the present invention:
Tebuconazole 93% (isomer 3%): 60g, saleratus: 5 grams, be warmed up to 120 ℃ of holding-zones, be incubated sampling in 3 o'clock, the tebuconazole 95.7% of survey; Isomer 0.1, epoxy 0.6%, with 150 grams, ethers and ethyl acetate class mixed solvent are purified then, and oven dry gets material 49.8 grams, and content is 97.0%.
The comparative example 3
Former technology:
Tebuconazole 93% (isomer 3%): 60g, caustic soda: 5 grams, be warmed up to 120 ℃ of holding-zones, be incubated sampling in 5 hours, tebuconazole is 82.5%, and isomer is 0.05%, and epoxy is 12.6%; Purify with 150 gram ethers and ethyl acetate class mixed solvent then, oven dry gets material 40.2 grams, content is 96.3%.
Technology of the present invention:
Tebuconazole 93% (isomer 3%): 60g, saleratus: 5 grams, be warmed up to 120 ℃ of holding-zones, be incubated sampling in 5 o'clock, the tebuconazole 95.4% of survey; Isomer 0.05%, epoxy 0.4% is purified with 150 gram ethers and ethyl acetate class mixed solvent then, and oven dry gets material 50.1 grams, and content is 97.1%.
Can get from above-mentioned Comparative Examples: after adding caustic soda, along with change of time, tebuconazole can being reversed, and add weakly alkaline salt, and tebuconazole is difficult for being reversed, and has improved the yield of former medicine.
Claims (4)
1. a tebuconazole is removed the preparation method of isomer, at first to tebuconazole, and tebuconazole isomer mixed solvent, impurity blended; Oiliness, crystal analyse that the still that does not come out is residual to be handled, and step is following: in still is residual, add sour earlier; Make the residual salify of still, in salt, drop into the buck hydrolysis then, after hydrolysis is accomplished; Add solvent treatment, behind the drying materials that obtains, the content that records isomer is bigger than normal; It is characterized in that: in the above-mentioned tebuconazole that contains isomer, add the weakly alkaline salts substances, be warming up to 120 back insulations 1-5 hour, isomer is converted into tebuconazole.
2. a kind of tebuconazole according to claim 1 is removed the preparation method of isomer, and it is characterized in that: the structural formula of said isomer is:
3. a kind of tebuconazole according to claim 1 is removed the preparation method of isomer, and it is characterized in that: said weakly alkaline salts substances is a potassium class weakly alkaline salt, and said potassium class weakly alkaline salt is saleratus.
4. a kind of tebuconazole according to claim 1 is removed the preparation method of isomer, and it is characterized in that: said weakly alkaline salts substances: the mol ratio that contains the tebuconazole of isomer is 1: 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010517489.1A CN102442958B (en) | 2010-10-25 | 2010-10-25 | Preparation method of isomer-removed tebuconazole |
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| CN201010517489.1A CN102442958B (en) | 2010-10-25 | 2010-10-25 | Preparation method of isomer-removed tebuconazole |
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| Publication Number | Publication Date |
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| CN102442958A true CN102442958A (en) | 2012-05-09 |
| CN102442958B CN102442958B (en) | 2015-02-18 |
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| CN201010517489.1A Active CN102442958B (en) | 2010-10-25 | 2010-10-25 | Preparation method of isomer-removed tebuconazole |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710373A (en) * | 2015-03-06 | 2015-06-17 | 上海晓明检测技术服务有限公司 | Preparation method for high-purity cyproconazole isomer |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1760187A (en) * | 2005-11-08 | 2006-04-19 | 湖南大学 | Method for preparing Tebucomazole in high purity |
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2010
- 2010-10-25 CN CN201010517489.1A patent/CN102442958B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1760187A (en) * | 2005-11-08 | 2006-04-19 | 湖南大学 | Method for preparing Tebucomazole in high purity |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710373A (en) * | 2015-03-06 | 2015-06-17 | 上海晓明检测技术服务有限公司 | Preparation method for high-purity cyproconazole isomer |
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| CN102442958B (en) | 2015-02-18 |
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Owner name: RUDONG ZHONGYI CHEMICAL CO., LTD. Free format text: FORMER OWNER: NANTONG PEST AGROCHEMICAL CO., LTD. Effective date: 20150629 |
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Effective date of registration: 20150629 Address after: 226400 No. two, Haibin Road, Rudong Coastal Economic Development Zone, Nantong, Jiangsu, China Patentee after: As Dong Zhongyi Chemical Co., Ltd. Address before: 226500 fine chemical industry zone, Rugao Port Economic Development Zone, Jiangsu, Rugao Patentee before: Nantong Pest Agrochemical Co., Ltd. |