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Purification method of pyriproxyfen technical, product obtained by purification method and application of product

A purification method, the technology of pyriproxyfen, which is applied in the direction of organic chemistry, can solve the problems of high content of isomer impurities, insufficient product purity, low overall yield, etc., and achieve the effects of ensuring purity, facilitating precipitation, and simple operation

Pending Publication Date: 2020-11-10
JIANGSU ROTAM CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method described in this scheme is difficult to separate the isomer impurities and pyriproxyfen well, and the content of pyriproxyfen isomers in the purified product is relatively high, and the overall yield is low
[0012] Although the above-mentioned literature discloses some methods for separating and purifying the original drug of pyriproxyfen, there are still problems such as high separation cost, high content of isomer impurities in the separated product, and insufficient product purity. Therefore, it is necessary to develop a simple-to-operate The purification method of the crude product of pyriproxyfen is still of great significance

Method used

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  • Purification method of pyriproxyfen technical, product obtained by purification method and application of product
  • Purification method of pyriproxyfen technical, product obtained by purification method and application of product
  • Purification method of pyriproxyfen technical, product obtained by purification method and application of product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Purification method of pyriproxyfen crude product:

[0061] (1) Add 100 g of crude pyriproxyfen technical product with a purity of 87.5% into a flask containing 90 mL of xylene, then add 100 mL of tetrahydrofuran, heat to reflux at 45° C., filter to remove insoluble impurities, and obtain solution A;

[0062] (2) Cool the solution A obtained in step (1) to 25°C at a cooling rate of 2°C / min, then place it in an ice-water bath to continue cooling and crystallization until the crystals are completely precipitated, filter, and dry under reduced pressure to obtain Purified pyriproxyfen technical substance.

[0063] In this embodiment, 86 g of white crystals were purified, and through quantitative analysis by high performance liquid chromatography, the purity of the obtained purified pyriproxyfen technical substance was 98.7%, and the yield of the purification process was 97%.

Embodiment 2

[0065] Purification method of pyriproxyfen crude product:

[0066] (1) Add 100 g of crude pyriproxyfen technical product with a purity of 93% into a flask containing 90 mL of n-hexane, then add 100 mL of methanol, heat to reflux at 45° C., filter to remove insoluble impurities, and obtain solution A;

[0067] (2) Cool the solution A obtained in step (1) to 25°C at a cooling rate of 3°C / min, add 3g of pure pyriproxyfen, and then place it in an ice-water bath to continue cooling and crystallization until the crystals are completely precipitated, Filter and dry under reduced pressure to obtain the purified pyriproxyfen technical substance.

[0068] Purified in this example, 92.4 g of white crystals were obtained. Quantitative analysis by high performance liquid chromatography showed that the purity of the purified pyriproxyfen technical product was 99.2%, and the yield of the purification process was 98.5%.

Embodiment 3

[0070] In this example, the cooling rate of step (2) in Example 1 is replaced by 3.5° C. / min, and other conditions are completely the same as those in Example 1.

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Abstract

The invention relates to a pyriproxyfen technical material purification method, a product obtained by the pyriproxyfen technical material purification method and an application of the product. The pyriproxyfen technical material purification method is characterized in that after a pyriproxyfen technical material crude product is dissolved, the obtained solution dissolved with pyriproxyfen is subjected to fractional cooling, so the purity of the pyriproxyfen technical material is improved. The purity of the purified pyriproxyfen active compound obtained by the purification method is greater than or equal to 98%, and the yield of the purification process is greater than or equal to 96%.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method for purifying pyriproxyfen as an active drug, a product obtained therefrom and uses thereof. Background technique [0002] Pyroxyfen, also known as pyriproxyfen, is a class of alkylpyridine juvenile hormone chitin synthesis inhibitors created and developed by Sumitomo Chemical in 1983. It can be used to control houseflies, mosquitoes, Termites and other sanitary pests, and can also control agricultural pests such as Homoptera, Thysanoptera, and Lepidoptera. It is a type of high-efficiency, environmentally friendly, and low-toxic insecticide. Pyriproxyfen has systemic transfer activity affecting larvae hiding on the underside of leaves. [0003] The molecular formula of pyriproxyfen is as follows: [0004] [0005] U.S. Patent No. 4,751,225 protects the original drug of pyriproxyfen and the synthesis process of the compound. It uses p-phenoxyphenol to react wi...

Claims

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Application Information

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IPC IPC(8): C07D213/64
CPCC07D213/64
Inventor 罗昌炎詹姆斯·T·布里斯托
Owner JIANGSU ROTAM CHEM
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