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Preparation method of key intermediate K acid of chlorantraniliprole

A technology of chlorantraniliprole and intermediates, which is applied in the field of preparation of K acid, the key intermediate of chlorantraniliprole, can solve the problems of multiple impurities, low yield, harsh condition control, etc., and achieve good selectivity, The effect of high product purity and high ring-forming yield

Inactive Publication Date: 2021-02-05
ZHEJIANG AVILIVE CHEM CO LTD +1
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Problems solved by technology

Under the current process conditions, in the process of synthesizing the pyrazole ring, because there are more reaction sites between the hydrazine group on the pyridine ring and diethyl maleate, more impurities will be generated, which leads to the reaction of this step. The condition control of the method is relatively harsh, and the yield is not high, and the purity of the intermediate product is not ideal; in addition, in the subsequent reaction of oxidation to construct the aromatic ring, an excessive amount of inorganic peroxysalt needs to be used, which leads to a large amount of difficult-to-handle Waste salt is generated, leaving environmental hazards

Method used

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  • Preparation method of key intermediate K acid of chlorantraniliprole
  • Preparation method of key intermediate K acid of chlorantraniliprole
  • Preparation method of key intermediate K acid of chlorantraniliprole

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Embodiment Construction

[0012] A kind of preparation method of chlorantraniliprole key intermediate K acid:

[0013] 1. Add 142g (1mol) of ethyl acetylacrylate, 93g (1.5mol) of ethylene glycol, and 19g (0.1mol) of p-toluenesulfonic acid (containing a part of crystal water) to 350ml of toluene, The device was heated to reflux, and the dehydration reaction was about 6h. The gas chromatography detected that the reaction raw materials disappeared. After the reaction, cool to below 10°C, wash with 200ml×2 water and 200ml saturated brine, separate the organic layer, add sodium bicarbonate to dry, filter, wash the filter cake with a small amount of toluene, and combine several layers. Distilled under reduced pressure, evaporated to substantially constant weight, 179g of light yellow oily matter, the gas chromatography detection purity of this oily matter is about 95%, can be directly used in the next step reaction without further separation.

[0014] 2. Dissolve the above yellow oil in 450ml of absolute et...

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Abstract

The invention relates to a preparation method of a key intermediate K acid of chlorantraniliprole. The preparation method has the advantages of fewer reaction sites, less impurity generation and capability of realizing efficient, green and environment-friendly preparation of K acid. According to the method, ethyl acetoacrylate is used as a raw material and subjected to carbonyl protection, cyclization, deprotection, oxidation and bromination so as to finally prepare the K acid. The method has the advantages of high cyclization yield, good selectivity and high product purity.

Description

technical field [0001] The invention relates to a preparation method of K-acid, a key intermediate of chlorantraniliprole, which has fewer reaction sites, fewer impurities, and can realize high-efficiency, green and environment-friendly preparation of K-acid, and belongs to the field of synthesis of pesticide and insecticide intermediates. Background technique [0002] Chlorantraniliprole is a new anthranilic benzoyl insecticide launched by DuPont in 2007. Because of its excellent insecticidal effect, low toxicity to non-target organisms, and no cross-resistance with existing insecticides The product has achieved good sales performance in the field of insecticides once it was launched, and has been in a period of rapid market expansion in recent years. Its structural formula is as follows: [0003] [0004] Although the preparation method of chlorantraniliprole currently reported and disclosed is not uncommon, the route that can be applied to large-scale preparation with...

Claims

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Application Information

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IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 赵能选李兰杰胡晓峰王良良钱广朱杰朱红薇
Owner ZHEJIANG AVILIVE CHEM CO LTD
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