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Separation and purification method of pyriproxyfen

A technology for separation and purification of pyriproxyfen, which is applied in the field of separation and purification of pyriproxyfen, which can solve the problems of low product purity, small amount of one-time separation, and high operating costs

Inactive Publication Date: 2006-11-29
SHANGHAI INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In summary, the existing pyriproxyfen separation and purification technology has the following disadvantages: (1) silica gel chromatographic column separation, although the purity is high, but the amount of separation at one time is small and the operating cost is high; (2) conventional recrystallization method Separation, due to the similar physical and chemical properties of the impurities and the product pyriproxyfen, the purity of the product obtained by recrystallization is not high no matter whether a single solvent or a mixed solvent is used

Method used

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  • Separation and purification method of pyriproxyfen
  • Separation and purification method of pyriproxyfen
  • Separation and purification method of pyriproxyfen

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Put 30.0g (0.16mol) of p-phenoxyphenol, 2.7g (0.048mol) of potassium hydroxide and 100mL of water into a 250mL reaction flask, stir and heat to 40°C, add dropwise 18.4g (0.32mol) of propylene oxide, React at 40-60°C for 4h. The reaction mixture was cooled to room temperature and filtered to obtain 35-38 g of 1-(4-phenoxyphenoxy)-2-propanol.

[0019] Put the above 1-(4-phenoxyphenoxy)-2-propanol, 25.0g (0.45mol) potassium hydroxide and 100mL ethylene glycol diethyl ether into a 250mL reaction flask, stir and heat to 80°C, drop Add 20.5g (0.18mol) of 2-chloropyridine and react at 80-120°C for 4h. The reaction mixture was cooled to room temperature, filtered, washed with water, and the filtrate was evaporated to remove the solvent under reduced pressure to obtain 47.0 g of crude pyriproxyfen. Quantitatively determined by HPLC, the content of pyriproxyfen was 85.1%.

[0020] Heat and dissolve the crude pyriproxyfen with 50mL of ethyl acetate, add 50-450mL of methanol, ad...

Embodiment 2

[0022] Put 30.0g (0.16mol) of p-phenoxyphenol, 2.7g (0.048mol) of potassium hydroxide and 100mL of water into a 250mL reaction flask, stir and heat to 40°C, add dropwise 18.4g (0.32mol) of propylene oxide, React at 40-60°C for 4h. The reaction mixture was cooled to room temperature and filtered to obtain 35-38 g of 1-(4-phenoxyphenoxy)-2-propanol.

[0023] Put the above 1-(4-phenoxyphenoxy)-2-propanol, 25.0g (0.45mol) potassium hydroxide and 100mL ethylene glycol diethyl ether into a 250mL reaction flask, stir and heat to 80°C, drop Add 20.5g (0.18mol) of 2-chloropyridine and react at 80-120°C for 4h. The reaction mixture was cooled to room temperature, filtered, washed with water, and the filtrate was evaporated to remove the solvent under reduced pressure to obtain 45.6 crude pyriproxyfen. Quantitatively determined by HPLC, the content of pyriproxyfen was 85.7%.

[0024] Heat and dissolve the crude pyriproxyfen with 50mL of toluene, add 50-450mL of methanol, adjust the te...

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Abstract

A process for separating and purifying pyriproxyfen after reaction includes such steps as filtering, water washing to filtrate twice, vacuum recovery of solvent to obtain coarse pyriproxyfen, dissolving it in ethyl acetate or toluene, adding alcohol, removing impurities, cooling and crystallizing. Its purity reaches more than 98.5%.

Description

technical field [0001] The invention relates to a method for separating and purifying insecticides containing diphenyl ether groups, more specifically to a method for separating and purifying pyriproxyfen. Background technique [0002] Pyriproxyfen (pyriproxyfen), chemical name is 4-phenoxyphenoxy-(RS)-2-(2-pyridyloxy)propyl ether, molecular formula C 20 h 19 NO 3 , the molecular weight is 321.38, and the chemical structural formula is as follows: [0003] [0004] Pyroxyfen is an insect growth regulator with juvenile hormone activity, which can be used to prevent and control agricultural pests of Homoptera, Thysanoptera, Diptera, and Lepidoptera, except for high toxicity to cotton whitefly and greenhouse whitefly. In addition to its activity, it has a good control effect on agricultural pests such as pear yellow psyllid, red garden scale insect, green peach aphid, Spodoptera litura, potato beetle and other agricultural pests. The principle of action is to select insec...

Claims

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Application Information

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IPC IPC(8): C07D213/64A01N43/40
Inventor 高永红陆庆宁陶建伟金东元周祖兴
Owner SHANGHAI INSTITUTE OF TECHNOLOGY
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