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A kind of purification method of chlorantraniliprole

A technology of chlorantraniliprole and a purification method, which is applied in the field of purification of chlorantraniliprole, can solve the problems of less than 90%, low purification yield, large amount of solvent, etc., and achieves reduction of purification cost, high yield, The effect of small total solvent usage

Active Publication Date: 2021-02-02
LIER CHEM CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] CN107400114A discloses a method for purifying chlorantraniliprole by solvent crystallization, but the method has the following problems: (1) the purification yield is low, less than 90%; (2) the amount of solvent used is relatively large, at least 30% of the crude product Doubling amount (g / mL)
Therefore, the method has high cost and is not suitable for industrial production.

Method used

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  • A kind of purification method of chlorantraniliprole

Examples

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Comparison scheme
Effect test

Embodiment 1

[0046] In this example, 21 groups of experiments were carried out according to the following method. The specific operation was as follows: suspend 1.5 g of crude chlorantraniliprole in a benign solvent, heat and dissolve until the system is completely clear, then add a poor solvent, and keep the system in the state of In the dissolved state, heat it for crystallization for 1.5 hours after heating, stop heating, naturally cool down to 37°C for 2.5 hours, filter with suction, and dry to constant weight to obtain the purified chlorantraniliprole product.

[0047] The purification parameters and results of each experimental group are shown in Table 1:

[0048] Table 1

[0049]

[0050] It can be seen from the data in Table 1 that when the benign solvent is DMF, DMA, DMSO, dioxane or THF, the purity of the purified chlorantraniliprole product is high (>97%), and the effect of DMA is better , the yield is all higher than 80%, and the product purity is generally higher than 99%;...

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Abstract

The invention discloses a method for purifying chlorantraniliprole, which belongs to the technical field of chemical industry. Aiming at the technical problems of low product yield and purity and large amount of solvent used in the current purification of chlorantraniliprole, the present invention provides a purification method of chlorantraniliprole, comprising the following steps: dissolving the crude product of chlorantraniliprole In a good solvent, add a poor solvent, crystallize, and obtain purified chlorantraniliprole. The method of the present invention can obtain high-purity chlorantraniliprole with a high yield through the control of each parameter in the purification process, and the total solvent consumption is small, which is beneficial to large-scale production in the industry, and greatly reduces the chlorantraniliprole. Purification cost of formamide.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a purification method of chlorantraniliprole. Background technique [0002] Chlorantraniliprole is a broad-spectrum insecticide with a new type of o-formamidobenzamide chemical structure successfully developed by DuPont of the United States for the first time. It has strong insecticidal activity, excellent field performance, less toxicity to mammals, and good environmental compatibility. The compound has excellent control effects on Lepidoptera pests, acts on ryanodine receptors, has the characteristics of high efficiency, low toxicity, safety to non-target organisms, and no cross-resistance to existing insecticides, so it has attracted widespread attention. Attention, has a huge market prospect. First launched in 2008, it is mainly used for soybeans, fruits and vegetables, rice, cotton and corn. Chlorantraniliprole has been sold in more than 100 countries in the world,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 李栋宏曾伟何波姚中伟左翔程柯
Owner LIER CHEM CO LTD
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