CN102442958B - Preparation method of isomer-removed tebuconazole - Google Patents
Preparation method of isomer-removed tebuconazole Download PDFInfo
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- CN102442958B CN102442958B CN201010517489.1A CN201010517489A CN102442958B CN 102442958 B CN102442958 B CN 102442958B CN 201010517489 A CN201010517489 A CN 201010517489A CN 102442958 B CN102442958 B CN 102442958B
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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 the preparation method that a kind of tebuconazole removes isomer, specifically a kind of tebuconazole that can effectively prevent reversed reaction from producing removes the preparation method of isomer.
Background technology
Tebuconazole structural formula:
A kind of isomer can be generated in synthesis tebuconazole,
Isomer structure formula:
Farm crop, existing of isomer is nonsensical, and it consumes starting material, have impact on the content of tebuconazole, therefore isomer will be removed.
In original process, the conversion of isomer generally adds caustic soda, and when adding caustic soda conversion, General reactions speed is too fast, not too easily controls, 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, first to tebuconazole, tebuconazole isomer mixed solvent, impurity mixing, oiliness, the crystal still of can not analysing is out residual to be processed, step is as follows: first in still is residual, add acid, make the residual salify of still, then in salt, drop into buck hydrolysis, after being hydrolyzed, add solvent treatment, after the drying materials obtained, the content recording isomer is bigger than normal, it is characterized in that: add weakly alkaline salts substances in above-mentioned containing in the tebuconazole of isomer, insulation 1-5 hour after being warming up to 120, isomer is converted into tebuconazole.
Further, the structural formula of described isomer is:
Further, described weakly alkaline salts substances is potassium class weakly alkaline salt.
Further, described weakly alkaline salts substances: the mol ratio containing the tebuconazole of isomer is 1: 4.
The invention has the advantages that: adopt weakly alkaline salts substances, effectively reduce the reversal of reaction, improve yield.
Embodiment
Comparative example 1
Former technique:
Tebuconazole 93% (isomer 3%): 60g, sodium hydroxide: 5 grams, is warmed up to 120 DEG C of holding-zones, is incubated sampling in 1 hour, the tebuconazole 94.2% of survey, isomer 0.2%, epoxy 2.6%; Then purify with 150 grams of ethers and ethyl acetate class mixed solvent, dry, obtain material 48.1 grams, content is 97.1%.
Technique of the present invention:
Tebuconazole 93% (isomer 3%): 60g, saleratus: 5 grams, heats up 120 DEG C, is incubated sampling in 1 hour, the tebuconazole 95.5% of survey, isomer 0.2%, epoxy 0.55%; Then use 150 grams, ethers and ethyl acetate class mixed solvent are purified, and dry, obtain material 50 grams, content is 97.2%.
Comparative example 2
Former technique:
Tebuconazole 93% (isomer 3%): 60g, caustic soda: 5 grams, is warmed up to holding-zone 120 DEG C, and be incubated sampling in 3 hours, tebuconazole is 90.5%, and isomer is 0.05%, and epoxy is 6.0%; Then use 150 grams, ethers and ethyl acetate class mixed solvent are purified, and dry, obtain material 45.2 grams, content is 96.9%.
Technique of the present invention:
Tebuconazole 93% (isomer 3%): 60g, saleratus: 5 grams, is warmed up to holding-zone 120 DEG C, samples, the tebuconazole 95.7% of survey when being incubated 3; Isomer 0.1, epoxy 0.6%, then uses 150 grams, and ethers and ethyl acetate class mixed solvent are purified, and dry, obtain material 49.8 grams, content is 97.0%.
Comparative example 3
Former technique:
Tebuconazole 93% (isomer 3%): 60g, caustic soda: 5 grams, is warmed up to holding-zone 120 DEG C, and be incubated sampling in 5 hours, tebuconazole is 82.5%, and isomer is 0.05%, and epoxy is 12.6%; Then purify with 150 grams of ethers and ethyl acetate class mixed solvent, dry, obtain material 40.2 grams, content is 96.3%.
Technique of the present invention:
Tebuconazole 93% (isomer 3%): 60g, saleratus: 5 grams, is warmed up to holding-zone 120 DEG C, samples, the tebuconazole 95.4% of survey when being incubated 5; Isomer 0.05%, epoxy 0.4%, then purify with 150 grams of ethers and ethyl acetate class mixed solvent, dry, obtain material 50.1 grams, content is 97.1%.
Can obtain from above-mentioned comparative example: after adding caustic soda, along with the change of time, tebuconazole can being reversed, and add weakly alkaline salt, and tebuconazole is being reversed not easily, improves the yield of former medicine.
Claims (2)
1. the preparation method of a tebuconazole removal isomer, first to tebuconazole, tebuconazole isomer mixed solvent, impurity mixing, oiliness, the crystal still of can not analysing is out residual to be processed, step is as follows: first in still is residual, add acid, make the residual salify of still, then in salt, drop into buck hydrolysis, after being hydrolyzed, add solvent treatment, after the drying materials obtained, the content recording isomer is bigger than normal, it is characterized in that: add potassium class weakly alkaline salt saleratus in above-mentioned containing in the tebuconazole of isomer, 1-5 hour is incubated after being warming up to 120 DEG C, isomer is converted into tebuconazole.
2. a kind of tebuconazole according to claim 1 removes the preparation method of isomer, it is characterized in that: described potassium class weakly alkaline salt saleratus: the mol ratio containing the tebuconazole of isomer is 1: 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| 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 CN102442958A (en) | 2012-05-09 |
| CN102442958B true 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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| 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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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. |