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Method for preparing diflubenzuron serving as pesticide

A technology for preparing insecticides and diflubenzuron, which is applied in the field of preparation of insecticides, can solve the problems of high cost of preparation methods, unreasonable catalysts, and low synthesis yields, and achieve environmental friendliness, low cost, and reasonable synthesis processes Effect

Active Publication Date: 2011-09-14
LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The catalyst used in the preparation method of diflubenzuron in the prior art is unreasonable, so that the synthesis yield is low and the cost of the preparation method is high

Method used

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  • Method for preparing diflubenzuron serving as pesticide
  • Method for preparing diflubenzuron serving as pesticide

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Example 1. A method for preparing the insecticide diflubenzuron, the specific steps are as follows:

[0016] (1) Add an appropriate amount of aromatic compound solvent into a reaction kettle equipped with an exhaust gas treatment system, stirring, a condenser, a vent pipe, and a thermometer, cool to -15°C, and pass in phosgene for 0.5 hours; stop cooling, and add an appropriate amount The catalyst dimethylformamide; at the same time, continue to pass phosgene, and slowly drop into the solution composed of p-chloroaniline and aromatic compound solvent, the temperature is slowly raised to 20 ° C, and drop at 20 ~ 50 ° C, 0.5 ~ 2.0 hours After the addition is complete; after dropping, keep stirring at 20-50°C for 0.4 hours, stop passing phosgene; then add an appropriate amount of co-catalyst triethylenediamine and aromatic compounds to form a solution; slowly heat to 90°C, keep warm for 4 hours, and keep warm for 4 hours. , feed in nitrogen, purge off the remaining phosge...

Embodiment 2

[0018] Example 2. A method for preparing the insecticide diflubenzuron, the specific steps are as follows:

[0019] (1) Add an appropriate amount of aromatic compound solvent into a reaction kettle equipped with an exhaust gas treatment system, stirring, a condenser, a vent pipe, and a thermometer, cool to -30°C, and pass in phosgene for 2.0 hours; stop cooling and add a catalyst Dimethylformamide (accounting for about 1~5% of the mass of p-chloroaniline); at the same time, continue to pass phosgene, and slowly drop into the solution composed of p-chloroaniline and aromatic compound solvent, the temperature is slowly raised to 20 ° C, and in 20~50℃, within 0.5~2.0 hours, the dropwise addition is completed; after the dropping is completed, keep stirring below 20~50℃ for 1.0 hour, stop passing phosgene; then add an appropriate amount of co-catalyst triethylenediamine and aromatic compounds to form a solution; slowly Heating to 100°C and keeping it warm for 4.0 hours; blowing in...

Embodiment 3

[0021] Example 3. In the method for preparing the insecticide diflubenzuron described in Example 1 or 2: the mass ratio of the raw material p-chloroaniline to 2,6-difluorobenzamide is 1:1.0.

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Abstract

The invention discloses a method for preparing diflubenzuron serving as a pesticide. The method is characterized by comprising the following steps of: adding an aromatic compound solvent into a reaction kettle, cooling, introducing phosgene, adding an appropriate amount of dimethyl methanamide, dripping a p-chloroaniline solution and adding triethylene diamine serving as a catalyst promoter; raising the temperature, preserving heat and stirring; reacting to obtain a solution containing rubigan isocyanate and the aromatic compound solvent; and adding 2,6-difluorobenzamide after adding the aromatic compound solvent into another reaction kettle, raising temperature and dripping a p-chloroaniline isocyanate solution to obtain the diflubenzuron. In the method, dimethyl methanamide serving as acatalyst and triethylene diamine serving as the catalyst promoter are used in a reaction, so that the total yield of synthesized diflubenzuron is over 91 percent, and the purity of a diflubenzuron active compound is over 99 percent. The method has the advantages of reasonable synthesis process, low cost, high quality and environmental friendliness, is up to the international standard, and is moresuitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing an insecticide, in particular to a method for preparing the insecticide diflubenzuron. Background technique [0002] Diflubenzuron, also known as Dimetralin, Diflubenzuron No. 1, is a new type of insect growth regulator; the pure product is white crystal, and the original powder is white to light yellow crystalline powder, which is insoluble in water and hardly soluble in most organic compounds. solvent. It is relatively stable to light and heat, easy to decompose when encountering alkali, stable in acidic and neutral medium, highly toxic to crustaceans and silkworms, safe to humans, animals and other organisms in the environment, and is a low-toxic and pollution-free pesticide. Its insecticidal mechanism is completely different from conventional insecticides in the past, neither nerve agents nor cholinesterase inhibitors. Diflubenzuron is a benzoate-based phenylurea insecticide, and it is the same inse...

Claims

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Application Information

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IPC IPC(8): C07C275/54C07C273/18
Inventor 王耀良石卫兵
Owner LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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