CN101693700A - Synthesis method of benazolin - Google Patents
Synthesis method of benazolin Download PDFInfo
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- CN101693700A CN101693700A CN200910035872A CN200910035872A CN101693700A CN 101693700 A CN101693700 A CN 101693700A CN 200910035872 A CN200910035872 A CN 200910035872A CN 200910035872 A CN200910035872 A CN 200910035872A CN 101693700 A CN101693700 A CN 101693700A
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- China
- Prior art keywords
- benazolin
- reaction
- benzothiazolone
- grams
- wormwood
- 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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- Thiazole And Isothizaole Compounds (AREA)
Abstract
The invention relates to a synthesis method of benazolin, belonging to the technical field of production process of the benazolin as an agricultural herbicide. The generation of side products is controlled by adopting a low-temperature method, adding a catalyst as well as reducing the reaction temperature from 90-95 DEG C to 60-65 DEG C. By adopting the invention, the production safety is improved, the content of the benazolin reaches 98 percent, and the total yield is more than 80 percent.
Description
Technical field
The present invention relates to the synthesis technology field of agricultural herbicide benazolin.
Background technology
Benazolin is a kind of herbicide used in rape field that is widely used in, and report obtains benazolin with benzothiazolone, salt of wormwood, ethyl chloroacetate reaction at present, and temperature of reaction is in 90～95 ℃ of scopes, and total recovery has only 60%, and content reaches 96%.Because highly energy-consuming, the yield of existing benazolin production technique are low, be unfavorable for that reducing disappears to sell cost, influenced and promoted the use of.
Summary of the invention
The object of the invention is to invent a kind of synthetic method that improves reaction yield, improves the benazolin of reactant content.
The present invention drops into reaction kettle for reaction with benzothiazolone, salt of wormwood, ethyl chloroacetate and catalyzer potassiumiodide, and temperature of reaction is 60～65 ℃, through the washing postcooling, obtains benazolin.
The present invention with potassiumiodide as catalyzer, benzothiazolone, salt of wormwood and ethyl chloroacetate are reacted, temperature of reaction is reduced to 60～65 ℃ by 90～95 ℃, the generation of may command by product, improve production security, content reaches 98%, and total recovery is greater than 80%, the present invention is consumed energy low, is beneficial to save to produce.
The mass ratio that adds catalyzer potassiumiodide and benzothiazolone among the present invention is 4～6: 100, and the add-on of appropriate catalyst not only can not cause cost to increase to production, and can reach purpose of design.
The present invention drops into benzothiazolone, salt of wormwood, ethyl chloroacetate, catalyzer potassiumiodide earlier, and under fully stirring, temperature rises to 60～65 ℃, insulation reaction, and reaction finishes after washing, obtains benazolin.
Embodiment
Example 1: in the there-necked flask of 1000mL, add benzothiazolone 94.8 grams (0.5mol), salt of wormwood 77 grams, ethyl chloroacetate 400 grams, potassiumiodide 6 grams, stirred 30 minutes, be heated to 60～65 ℃, insulation reaction 4 hours, the mass concentration of benzothiazolone is less than 0.3% in the detection reaction system, termination reaction, wash, dry to such an extent that benazolin 131 restrains yield 95%, content 98.5%.
Example 2: in the there-necked flask of 1000mL, add benzothiazolone 94.8 grams (0.5mol), salt of wormwood 77 grams, ethyl chloroacetate 400 grams, potassiumiodide 5 grams, stirred 30 minutes, be heated to 60～65 ℃, reacted 5 hours, the mass concentration of benzothiazolone is less than 0.3% in the detection reaction system, termination reaction, wash, dry to such an extent that benazolin 132 restrains yield 95.5%, content 98.3%.
Example 3: in the there-necked flask of 1000mL, add benzothiazolone 94.8 grams (0.5mol), salt of wormwood 77 grams, ethyl chloroacetate 400 grams, potassiumiodide 4 grams, stirred 30 minutes, be heated to 60～65 ℃, reacted 6 hours, the mass concentration of benzothiazolone is less than 0.3% in the detection reaction system, termination reaction, wash, dry to such an extent that benazolin 131 restrains yield 95.1%, content 98.6%.
Example 4: in the there-necked flask of 1000mL, add benzothiazolone 94.8 grams (0.5mol), salt of wormwood 77 grams, ethyl chloroacetate 400 grams stirred 30 minutes, were heated to 80～85 ℃, reacted 6 hours, the mass concentration of benzothiazolone is less than 0.3% in the detection reaction system, and termination reaction is washed, dries to such an extent that benazolin 129 restrains, yield 92.1%, content 95.6%.
Claims (2)
1. the synthetic method of a benazolin drops into reaction kettle for reaction with benzothiazolone, salt of wormwood and ethyl chloroacetate, it is characterized in that adding the catalyzer potassiumiodide when reaction, and temperature of reaction is 60～65 ℃, through the washing postcooling, obtains benazolin.
2. according to the synthetic method of the described benazolin of claim 1, it is characterized in that the catalyzer potassiumiodide that adds and the mass ratio of benzothiazolone are 4～6: 100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910035872A CN101693700A (en) | 2009-10-09 | 2009-10-09 | Synthesis method of benazolin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910035872A CN101693700A (en) | 2009-10-09 | 2009-10-09 | Synthesis method of benazolin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101693700A true CN101693700A (en) | 2010-04-14 |
Family
ID=42092710
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910035872A Pending CN101693700A (en) | 2009-10-09 | 2009-10-09 | Synthesis method of benazolin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101693700A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116003344A (en) * | 2022-06-14 | 2023-04-25 | 内蒙古工业大学 | Method for preparing pesticide herb ethyl ester by utilizing carbon dioxide and o-amino sulfide and product thereof |
-
2009
- 2009-10-09 CN CN200910035872A patent/CN101693700A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116003344A (en) * | 2022-06-14 | 2023-04-25 | 内蒙古工业大学 | Method for preparing pesticide herb ethyl ester by utilizing carbon dioxide and o-amino sulfide and product thereof |
| CN116003344B (en) * | 2022-06-14 | 2024-04-12 | 内蒙古工业大学 | Method for preparing pesticide herb ethyl ester by utilizing carbon dioxide and o-amino sulfide and product thereof |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20100414 |