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Purification method of non-fatty oxime ether pyrethrin compound

A kind of technology of oxime etherethrin and purification method, applied in the directions of oxime preparation, organic chemistry, etc., can solve the problems of complicated process, low product yield, difficult to handle and the like

Inactive Publication Date: 2007-09-19
HUNAN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the purification method of non-esteroxime ether chrysanthemum esters is usually separated and purified by vacuum column chromatography, which is not only complicated in process, but also consumes a lot of solvents, low product yield, high cost, large amount of three wastes, and is not easy to handle.

Method used

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  • Purification method of non-fatty oxime ether pyrethrin compound
  • Purification method of non-fatty oxime ether pyrethrin compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Purification of isopropyl-4-chlorophenone oxime-O-(3-phenoxybenzyl) ether

[0013] In a 500mL three-necked flask equipped with a stirring and thermometer, add 100g of industrial product of isopropyl-4-chlorophenoneoxime-O-(3-phenoxybenzyl)ether with a purity of 66.3%, petroleum ether: methanol : Methyl formate=9:6:0.9 mixed solvent 200mL, after stirring and mixing, put it in a low temperature bath, and cool for 8 hours at 0℃~-15℃. filter. The crystals were washed with cold petroleum ether, and dissolved under reduced pressure to obtain 65.85 g of a product with a purity of 95.6% and a yield of 82.5%.

Embodiment 2

[0015] Purification of 1-(4-chlorophenyl)-2-methylthio-O-[(3-phenoxyphenyl)methyl]acetone oxime ether 76.25% 1-(4-chlorophenyl)-2-methylthio-O-[(3-phenoxyphenyl)methyl]acetone oxime ether industrial product 115.7g, petroleum ether: absolute ethanol: ethyl acetate Ester=3:1:0.3 mixed solvent 230mL, after stirring evenly, put it in a low temperature bath, and cool for 24 hours at -10℃~-15℃. filter. The crystals were washed with cold petroleum ether, and dissolved under reduced pressure to obtain 76.4 g of a product with a purity of 96.1% and a yield of 83.22%.

Embodiment 3

[0017] Purification of 5-chloro-3-methyl-1-phenylpyrazole-4-carbaldehyde oxime-O-2-chloro-5-pyridyl methyl ether

[0018] In a 500 mL three-neck flask equipped with a stirring and thermometer, add 100 g of the above title compound with a purity of 65.1%, 200 mL of petroleum ether: isopropanol: isobutyl acetate = 6: 3:1 mixed solvent, and after stirring, put it in Cool in a low temperature bath at -15℃~-25℃ for 16 hours. filter. The crystals were washed with cold petroleum ether, and dissolved under reduced pressure to obtain 64.7 g of a product with a purity of 95.3% and a yield of 82.1%.

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PUM

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Abstract

The invention discloses a purifying method represented by formula (I) for non-ester oxime-ether pyrethroid, including dissolving the low amount of composition (formula I) in the mixing solvent at 5-35 DGE C; cooling and crystallizing at 0-25 DEG C; filtering and precipitating after 8-24 hours; then getting the oxime-ether composition with a content >=95%. The invention has a good selectivity, a large disposal amount, a less pollution, simple art, a convenient operation and chooses a cheap solvent, can effectively removes the impurities and improves the low amount coarse product more than 95%.

Description

Technical field [0001] The present invention relates to a method for purifying non-ester oxime ether pyrethroid compounds. Background technique [0002] Chinese patent CN1159290C discloses the biological activity and preparation method of the general chemical structure of non-ester oxime ether pyrethroid compounds. The non-ester oxime ether pyrethroid compounds have excellent biological activity in insecticidal, and have a wide insecticidal spectrum, rapid action, safety to natural enemies and crops, and good environmental compatibility. At present, it has been applied to a variety of crops such as rice, vegetables, and fruit trees. However, due to the long synthetic route of this kind of compound, many side reactions, many impurities in the crude product, and similar properties, the separation is very difficult, and the effective ingredients are generally ≤76%. If the product with this content is applied to crops, it will not only reduce the efficacy of the medicine, increase th...

Claims

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Application Information

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IPC IPC(8): C07C251/50C07C249/14
Inventor 王晓光陈九星吴光群段湘生王洪成陈明聂萍陈力华
Owner HUNAN CHEM RES INST
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