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Preparation method of cycloxaprid

A technology of cyclofenapyr and sodium hydroxide, applied in the direction of organic chemistry and the like, can solve problems such as low purity of cyclofenapyr, and achieve the effects of good application prospect and economic benefit, safe preparation method and high purity

Inactive Publication Date: 2021-04-16
NANTONG TENDENCI CHEM
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Problems solved by technology

[0008] In the process of using 2-chloro-5-chloromethylpyridine, succinaldehyde and imidazolidine to generate cyclopyrid, due to side reactions in the reaction, the purity of cyclopyrid in the final product is relatively low

Method used

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  • Preparation method of cycloxaprid
  • Preparation method of cycloxaprid

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Embodiment Construction

[0020] The technical solution of the present invention will be further described below in conjunction with the examples. The technical schemes and related parameters given in the following embodiments are only exemplary, and are intended to explain the present invention, but should not be construed as limiting the present invention.

[0021] This embodiment discloses a preparation method of cyclopyridam, in which the addition process of each component is carried out by dropping, and the specific steps are as follows:

[0022] 1) Add 100g of clear water, 70g of nitroguanidine with a water content of 25%, and 24.5g of concentrated sulfuric acid into a 500ml round-bottomed flask. After stirring evenly, add 33g of ethylenediamine dropwise, heat up to 70°C, keep warm for 1h, and cool down after the reaction is completed. Filtrating, washing, collecting and drying the filter cake to obtain 2-nitroiminoimidazolidine, and the filtrate is concentrated and used mechanically;

[0023] 2...

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Abstract

The invention provides a preparation method of cycloxaprid, which comprises the following steps: synthesizing an intermediate 1 from nitro-guanidine and ethylene diamine under the catalytic action of concentrated sulfuric acid, reacting the intermediate 1 with caustic soda liquid and formaldehyde to generate an intermediate 2, nitrifying the intermediate 2 to obtain an intermediate 3, reacting the intermediate 3 with 2-chloro-5-chloromethyl pyridine and butanedial under the action of a catalyst aluminum trichloride to obtain a product namely cycloxaprid, and carrying out post-treatment: cooling, filtering, washing and drying to obtain a cycloxaprid solid. The prepared cycloxaprid product is high in purity and low in impurity content, and the yield of cycloxaprid in the final product can reach 50% or above; the used solvent chloroform can be recycled, and the recovery rate is 75% or above; the raw materials are low in pollution, and the preparation method is safe, environmentally friendly, suitable for large-scale industrial production and good in application prospect and economic benefit.

Description

technical field [0001] The invention relates to a preparation method of cyclopyridam, which belongs to the technical field of organic synthesis. Background technique [0002] Cyclopyrid is a cisnitronyl oxygen-bridged heterocyclic neonicotinoid insecticide with the molecular formula C 14 h 15 ClN 4 o 3 , the chemical structural formula is as follows: [0003] [0004] Cyclopyrid is a white or light yellow powder solid in macroscopic view, odorless, melting point 149.0-50.0°C, soluble in dichloromethane and chloroform, slightly soluble in water and ethanol. Cyclopyrid stability: hydrolysis half-life DT 50 : 5.03h (25°C, pH=4), 64.18h (25°C, pH=7), 577.62h (25°C, pH=9); photolysis half-life in water DT 50 =7.61min[(25±1)°C, pH=7, 300W high-pressure mercury lamp, 10cm away from the light source]. The photostability of cyclopyrid in water is lower than that of piperid, but better than that of imidacloprid. [0005] Cyclopyrid is the first highly active neonicotinoid r...

Claims

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Application Information

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IPC IPC(8): C07D498/18
Inventor 曹文军
Owner NANTONG TENDENCI CHEM
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