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Synthesis method of chlorantraniliprole

A technology of chlorantraniliprole and a synthesis method, applied in the field of chlorantraniliprole synthesis, can solve the problems of high pyridine recovery and waste water treatment costs, reduce waste water generation and processing difficulty, improve yield, and increase economic effect

Pending Publication Date: 2022-01-07
江西汇和化工有限公司
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Problems solved by technology

[0003] Find according to retrieval, the Chinese patent that the patent No. is CN_101072767_A discloses the method for preparing N-phenylpyrazole-1-carboxamide, and it uses 3-bromo-1-(3-chloro-2-pyridyl)-1 hydrogen- Chlorantraniliprole (3-bromo-N-[4-chloro-2-methyl-6- (Methylcarbamoyl) benzene]-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxamide), using reagents such as pyridine, methanesulfonyl chloride, acetonitrile, a large amount of pyridine-containing , sodium chloride, sodium methanesulfonate to obtain high-salt wastewater, pyridine recovery and wastewater treatment costs are very high

Method used

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  • Synthesis method of chlorantraniliprole

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Embodiment

[0017] Embodiment: a kind of synthetic method of chlorantraniliprole, comprises the following steps,

[0018] Step 1, prepare the 1000ml four-neck flask that is equipped with mechanical stirrer, thermometer and condenser earlier, add 3-bromo-1-(3-chloro-2-pyridyl)-1 hydrogen-pyrazole-5-carboxylic acid ( Purity 98.5%, 100g, 0.298mol), toluene 600ml and DMF (purity 99%, 0.5g, 0.007mol), stir well;

[0019] Step 2, add triphosgene (purity 99%, 100g, 0.334mol) during the stirring process, heat up to 70-110°C, a large amount of gas is generated, keep warm until the system is dissolved, and obtain 3-bromo-1-(3 -Chloro-2-pyridyl)-1 hydrogen-pyrazole-5-formyl chloride toluene solution;

[0020] Step 3, add 2-amino-5-chloro-N,3-methylbenzene to 3-bromo-1-(3-chloro-2-pyridyl)-1 hydrogen-pyrazole-5-formyl chloride toluene solution Formamide (purity 97.0%, 63.9g, 0.313mol) was heated to reflux, and after 5 hours of reflux reaction, the reaction was completed, and the temperature was low...

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Abstract

The invention discloses a synthesis method of chlorantraniliprole, and relates to the field of synthesis of pesticide chlorantraniliprole. The synthesis method comprises the following steps: step 1, firstly preparing a four-neck flask, adding 3-bromo-1-(3-chloro-2-pyridyl)-1-hydro-pyrazole-5-formic acid, and uniformly conducting stirring. The method takes 3-bromo-1-(3-chloro-2-pyridyl)-1-hydro-pyrazole-5-formic acid as an initial raw material, adopts an acylating chlorination reagent and takes methylbenzene, acetonitrile or dichloroethane (preferably methylbenzene) as a solvent, acylating chlorination reaction is conducted to synthesize an acyl chloride methylbenzene solution of the acid, and 2-amino-5-chloro-N,3-dimethylbenzamide is added into the acyl chloride methylbenzene solution without separation, and reflux reaction is conducted to obtain a chlorantraniliprole product. According to the present invention, the yield of the chlorantraniliprole produced by using the method is substantially improved, the wastewater generation amount and the treatment difficulty are reduced, the production quality is improved, the economic benefits are increased, and the large-scale production is easily achieved.

Description

technical field [0001] The invention relates to the field of synthesizing the pesticide chlorantraniliprole, in particular to a method for synthesizing chlorantraniliprole. Background technique [0002] The pesticide residues in agricultural products and the toxicity to animals have always been a hot spot of concern. In recent years, DuPont has successfully developed various high-efficiency and low-toxicity pesticides, which are changing the impact of pesticides on the environment. Insecticide research and development successfully led to chlorantraniliprole. Chlorantraniliprole has strong permeability and systemic conductivity. The pesticide that enters the plant is transmitted along the xylem to other parts that have not been applied, which is beneficial to the protection of newborn tissues. ; Stomach toxicity is the main type, followed by contact action; long-lasting effect, resistant to rain erosion. [0003] Find according to retrieval, the Chinese patent that the paten...

Claims

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Application Information

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IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 尹旺华李辉虎刘洋孙国强谢林涛姜永亮饶云会
Owner 江西汇和化工有限公司
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