CN102174013A - New synthesis technology of acetamiprid - Google Patents
New synthesis technology of acetamiprid Download PDFInfo
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- CN102174013A CN102174013A CN2011100571305A CN201110057130A CN102174013A CN 102174013 A CN102174013 A CN 102174013A CN 2011100571305 A CN2011100571305 A CN 2011100571305A CN 201110057130 A CN201110057130 A CN 201110057130A CN 102174013 A CN102174013 A CN 102174013A
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- acetamiprid
- synthesis technology
- new synthesis
- cyano group
- methyl alcohol
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Abstract
The invention relates to a new synthesis technology of acetamiprid used as agricultural insecticide. The new synthesis technology comprises the following steps: benzylmethylamine and ethyl N-cyanoethanimideate are added in a flask provided with a stirrer, a thermometer and a tail gas absorption device, under the condition that methanol is used as solvent, the temperature is heated to 65 DEG C to react for 5 hours; and acetone is used to elute and obtain acetamiprid. In the new synthesis technology, the weight ratio of benzylmethylamine to ethyl N-cyanoethanimideate is 150:110; and the synthesis yield can be increased from 90% to 95%, and the product purity can be increased from 96% to 98%.
Description
Technical field
The present invention relates to agricultural insecticide acetamiprid new synthesis technology.
Background technology
Acetamiprid is a kind of New-type wide-spectrum and sterilant with certain acaricidal activity, and its mode of action is system's sterilant of soil and branches and leaves.Be widely used in
Paddy rice, especially vegetables,
Fruit tree, tealeaves
Aphid, plant hopper,
Thrips, lepidopteran etc.
InsectControl, preventive effect is more than 90%.At present the operational path of report mainly is being raw material with 2-chloro-5-chloromethylpyridine, is to react under the condition of solvent at ethanol with Monomethylamine, obtains N-(6-chloro-3-picolyl) methylamine, then with the acetamiprid of N-cyano group second imido acid ethyl ester reaction.
Summary of the invention
The object of the invention is to invent a kind of new technology with N-cyano group second imido acid methyl esters synthetic acetamiprid under the condition of replacement N-cyano group second imido acid ethyl ester at alcohol solvent under the condition of methanol solvate, and product yield and quality are improved.
Technical scheme of the present invention is: the present invention adds benzyl methylamine and N-cyano group second imido acid methyl esters in the flask that stirring, thermometer and device for absorbing tail gas are housed, be under the condition of solvent with methyl alcohol, be warming up to 65 ℃, reacting 5 hours, use acetone drip washing, get acetamiprid.
Described benzyl methylamine is a raw material with 2-chloro-5-chloromethylpyridine, is to react under the condition of solvent to make at methyl alcohol with Monomethylamine.
Described benzyl methylamine and N-cyano group second imido acid methyl esters weight ratio are 150: 110-150.
Described benzyl methylamine and methyl alcohol weight ratio are 150: 100.
After testing, benzyl methylamine and N-cyano group second imido acid methyl esters weight ratio are 150: 110 among the present invention, can guarantee that synthesis yield 90% brings up to 95%, and product purity brings up to 98% from 96%.
Embodiment
Example is equipped with and adds 150 gram benzyl methylamines and N-cyano group second imido acid methyl esters 110 grams in the 1000ml four-hole boiling flask of stirring, thermometer and device for absorbing tail gas at 1: one, add methyl alcohol 100 grams, be warming up to 60 ℃, reacted 5 hours, sampling benzyl methylamine transformation efficiency 99.8%, cooling is filtered, crystal acetone drip washing, get acetamiprid yield 95%, product purity 98%.
Example is equipped with and adds 150 gram benzyl methylamines and N-cyano group second imido acid methyl esters 110 grams in the 1000ml four-hole boiling flask of stirring, thermometer and device for absorbing tail gas at 2: one, add methyl alcohol 100 grams, be warming up to 65 ℃, reacted 5 hours, sampling benzyl methylamine transformation efficiency 96.4%, cooling is filtered, crystal acetone drip washing, get acetamiprid yield 90%, product purity 94%.
Example is equipped with and adds 150 gram benzyl methylamines and N-cyano group second imido acid methyl esters 150 grams in the 1000ml four-hole boiling flask of stirring, thermometer and device for absorbing tail gas at 3: one, add methyl alcohol 100 grams, be warming up to 60 ℃, reacted 5 hours, sampling benzyl methylamine transformation efficiency 98%, cooling is filtered, crystal acetone drip washing, get acetamiprid yield 92%, product purity 95%.
Example is equipped with and adds 150 gram benzyl methylamines and N-cyano group second imido acid methyl esters 110 grams in the 1000ml four-hole boiling flask of stirring, thermometer and device for absorbing tail gas at 4: one, add methyl alcohol 100 grams, be warming up to 60 ℃, reacted 10 hours, sampling benzyl methylamine transformation efficiency 99%, cooling is filtered, crystal acetone drip washing, get acetamiprid yield 94.8%, product purity 98%.
It is raw material that above-mentioned benzyl methylamine preferentially adopts with 2-chloro-5-chloromethylpyridine, is to react under the condition of solvent to make at methyl alcohol with Monomethylamine, to guarantee that whole reflection efficient is effectively guaranteed.
Claims (4)
1. the acetamiprid new synthesis technology is characterized in that, adds benzyl methylamine and N-cyano group second imido acid methyl esters in the flask that stirring, thermometer and device for absorbing tail gas are housed, be under the condition of solvent with methyl alcohol, be warming up to 65 ℃, reacting 5 hours, use acetone drip washing, get acetamiprid.
2. acetamiprid new synthesis technology according to claim 1 is characterized in that, described benzyl methylamine is a raw material with 2-chloro-5-chloromethylpyridine, is to react under the condition of solvent to make at methyl alcohol with Monomethylamine.
3. acetamiprid new synthesis technology according to claim 1 is characterized in that, described benzyl methylamine and N-cyano group second imido acid methyl esters weight ratio are 150: 110-150.
4. acetamiprid new synthesis technology according to claim 3 is characterized in that, described benzyl methylamine and methyl alcohol weight ratio are 150: 100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100571305A CN102174013A (en) | 2011-03-10 | 2011-03-10 | New synthesis technology of acetamiprid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100571305A CN102174013A (en) | 2011-03-10 | 2011-03-10 | New synthesis technology of acetamiprid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102174013A true CN102174013A (en) | 2011-09-07 |
Family
ID=44517311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100571305A Pending CN102174013A (en) | 2011-03-10 | 2011-03-10 | New synthesis technology of acetamiprid |
Country Status (1)
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| CN (1) | CN102174013A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610135A (en) * | 2014-02-21 | 2015-05-13 | 江苏克胜作物科技有限公司 | Method for treating acetamiprid crystallization mother liquor |
| CN104803910A (en) * | 2015-03-26 | 2015-07-29 | 江苏长青农化南通有限公司 | Production process of acetamiprid |
| CN106187868A (en) * | 2016-07-15 | 2016-12-07 | 南通天泽化工有限公司 | A kind of preparation method of Acetamiprid |
| CN109061158A (en) * | 2018-09-21 | 2018-12-21 | 中国烟草总公司郑州烟草研究院 | A kind of time-resolved fluoroimmunoassay chromatograph test strip and its preparation method and application detecting Acetamiprid |
| CN114605319A (en) * | 2020-12-09 | 2022-06-10 | 南通天泽化工有限公司 | Preparation method of acetamiprid |
-
2011
- 2011-03-10 CN CN2011100571305A patent/CN102174013A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610135A (en) * | 2014-02-21 | 2015-05-13 | 江苏克胜作物科技有限公司 | Method for treating acetamiprid crystallization mother liquor |
| CN104610135B (en) * | 2014-02-21 | 2017-07-28 | 江苏克胜作物科技有限公司 | A kind of method for handling Acetamiprid crystalline mother solution |
| CN104803910A (en) * | 2015-03-26 | 2015-07-29 | 江苏长青农化南通有限公司 | Production process of acetamiprid |
| CN106187868A (en) * | 2016-07-15 | 2016-12-07 | 南通天泽化工有限公司 | A kind of preparation method of Acetamiprid |
| CN109061158A (en) * | 2018-09-21 | 2018-12-21 | 中国烟草总公司郑州烟草研究院 | A kind of time-resolved fluoroimmunoassay chromatograph test strip and its preparation method and application detecting Acetamiprid |
| CN114605319A (en) * | 2020-12-09 | 2022-06-10 | 南通天泽化工有限公司 | Preparation method of acetamiprid |
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| PB01 | Publication | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110907 |