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Method for preparing 4-(4-methylphenoxy) benzylamine through catalysis of modified nano nickel

A technology of methylphenoxy and nano-nickel, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc., can solve problems such as low product purity, high production cost, and poor preparation efficiency, and achieve The effect of simple process route, low production cost and high production efficiency

Inactive Publication Date: 2022-05-31
南京科力硕生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 4-(4-methylphenoxy)benzylamine is a key intermediate for the synthesis of pyrenpyrrole, although there are many reports on the method of synthesizing 4-(4-methylphenoxy)benzylamine, but These methods generally have problems such as the use of a large amount of highly toxic reagents, unstable hydrogenation catalysis, poor repeatability, long process routes, high production costs, and low product yields.
This method has the advantages of simple process, easy separation, and not easy to oxidize, but the preparation efficiency is poor, the product purity is not high, and the requirements for grinding equipment are relatively high.

Method used

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  • Method for preparing 4-(4-methylphenoxy) benzylamine through catalysis of modified nano nickel
  • Method for preparing 4-(4-methylphenoxy) benzylamine through catalysis of modified nano nickel
  • Method for preparing 4-(4-methylphenoxy) benzylamine through catalysis of modified nano nickel

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1 Utilizes the method for synthesizing 4-(4-methylphenoxy)benzylamine catalyzed by modified nano-nickel:

[0032] (1) Add 1 L of water, 60 g of nickel chloride, and 10 g of Span-20 into a beaker, stir and mix, add 10 g of sodium borohydride, adjust the pH to 10 with 1 mol / L sodium hydroxide solution, and carry out Ultrasonic treatment, the ultrasonic power is 1000 W, and the reaction time is 30 min. After the reaction, the modified nano-nickel is obtained after centrifugation, washing and drying;

[0033] (2) Add 1 L of water, 1.5 kg of potassium hydroxide, 2.5 kg of p-cresol, and 10 L of dimethyl sulfoxide into the reaction kettle, stir and mix and heat to 150°C, then add 3 kg of p-chlorobenzonitrile, continue Stir the reaction, finish the reaction after 3 h of reaction, recover the organic solvent, add water to cool down to room temperature, and then filter, wash and dry the reaction solution to obtain 4-(4-methylphenoxy)benzonitrile;

[0034] (3) In the a...

Embodiment 2

[0035] Embodiment 2 Utilizes the method for synthesizing 4-(4-methylphenoxy)benzylamine catalyzed by modified nano-nickel:

[0036] (1) Add 1 L of water, 60 g of nickel chloride, and 10 g of Span-60 into a beaker, stir and mix, add 10 g of sodium cyanoborohydride, and adjust the pH to 10 with 1 mol / L sodium hydroxide solution. And carry out ultrasonic treatment, the ultrasonic power is 1500 W, and the reaction time is 30 min. After the reaction, the modified nano-nickel is obtained after centrifugation, washing and drying;

[0037] (2) Add 1 L of water, 1.5 kg of potassium hydroxide, 2.5 kg of p-cresol, and 10 L of dimethyl sulfoxide into the reaction kettle, stir and mix and heat to 150°C, then add 3 kg of p-chlorobenzonitrile, continue Stir the reaction, finish the reaction after 3 h of reaction, recover the organic solvent, add water to cool down to room temperature, and then filter, wash and dry the reaction solution to obtain 4-(4-methylphenoxy)benzonitrile;

[0038] (3)...

Embodiment 3

[0039] Embodiment 3 Utilizes the method for synthesizing 4-(4-methylphenoxy)benzylamine catalyzed by modified nano-nickel:

[0040](1) Add 1 L of ethanol, 50 g of nickel nitrate, and 20 g of Span-20 into a beaker, stir and mix, add 10 g of sodium borohydride, adjust the pH to 10 with 1 mol / L sodium hydroxide solution, and perform ultrasonication treatment, the ultrasonic power was 1000 W, and the reaction time was 60 min. After the reaction, the modified nano-nickel was obtained after centrifugation, washing and drying;

[0041] (2) Add 1 L of water, 1.5 kg of potassium hydroxide, 2.5 kg of p-cresol, and 10 L of toluene into the reaction kettle, stir and mix and heat to 150°C, then add 3 kg of p-chlorobenzonitrile, continue to stir and react, and react After 3 h, the reaction was terminated, the organic solvent was recovered, the temperature was lowered to room temperature by adding water, and the reaction solution was filtered, washed and dried to obtain 4-(4-methylphenoxy)be...

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Abstract

The invention belongs to the field of synthesis of pesticide intermediates, and provides a method for catalytically synthesizing 4-(4-methylphenoxy) benzylamine by utilizing modified nano nickel. The preparation method specifically comprises the following steps: (1) stirring and mixing a solvent, a metal nickel salt, a polyhydric alcohol type nonionic surfactant, a reducing agent and an alkali solution, and performing ultrasonic treatment to prepare modified nano nickel; (2) adding water, potassium hydroxide, p-cresol, an organic solvent and p-chlorobenzonitrile into a reaction kettle, and stirring for reaction to prepare 4-(4-methylphenoxy) benzonitrile; and (3) adding ammonia water, ethanol, the modified nano nickel and 4-(4-methylphenoxy) benzonitrile into a high-pressure kettle, and introducing hydrogen to prepare the 4-(4-methylphenoxy) benzylamine. Compared with the prior art, the modified nano nickel catalyst used in the invention has the advantages of small particle size, high catalytic efficiency, good reusability and the like, and the production efficiency of the product is improved.

Description

technical field [0001] The invention belongs to the field of synthesis of pesticide intermediates, and in particular relates to a method for preparing 4-(4-methylphenoxy)benzylamine by using modified nano-nickel to catalyze. Background technique [0002] In recent years, heterocyclic insecticides and acaricides have become one of the important research hotspots in the field of insecticides. Among them, pyrazole insecticides and acaricides have the advantages of safety, high efficiency, low toxicity, no cross-resistance, and unique mechanism of action. , has become an important component of heterocyclic insecticides. As a new type of pyrazole heterocyclic insecticide and acaricide, its main mechanism of action is to prevent the oxidative phosphorylation of insects, and it also has the functions of killing eggs, inhibiting feeding, inhibiting oviposition and bactericidal. [0003] 4-(4-methylphenoxy)benzylamine is a key intermediate for the synthesis of pyrenpyrrole, although...

Claims

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Application Information

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IPC IPC(8): C07C213/02C07C217/58B01J23/755B01J31/02
CPCC07C213/02C07C253/30B01J23/755B01J31/0209B01J2231/641C07C217/58C07C255/54Y02P20/584
Inventor 许晖曹逊钱琦
Owner 南京科力硕生物科技有限公司
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