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Process for preparing Grignard reagent benzyl magnesium chloride by phonochemical method

A technology of Grignard reagent and benzylmagnesium chloride, applied in the direction of magnesium organic compounds, etc., can solve the problems of inconvenient industrial production of Grignard reagent, harsh environmental requirements, etc., and achieve the effects of low cost, easy industrialization, and high yield

Inactive Publication Date: 2006-03-22
GUANGDONG UNIV OF TECH
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Problems solved by technology

The traditional process is usually difficult at the beginning of the reaction, and an initiator needs to be added for the reaction to occur. The reaction requires extremely high purity of the solvent. Generally, AR-grade solvents must be specially treated to meet the requirements, and the environmental requirements are harsh. Oxygen, these all bring greater inconvenience to the industrial production of Grignard reagents

Method used

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  • Process for preparing Grignard reagent benzyl magnesium chloride by phonochemical method

Examples

Experimental program
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Effect test

example 1

[0033] Example 1: Simply evacuate the dry four-necked flask with nitrogen, then put 10g of fresh Mg, 24ml of benzyl chloride, and 240ml of ether into the four-necked flask, mix them evenly, and place them in an ultrasonic device for ultrasonic reaction. Within 10 minutes, the reaction was initiated, and the reaction ended in 10 minutes. During this period, attention should be paid to the intensity of the reaction, and part of the heat of reaction should be removed in time. After the reaction was completed, the reaction was refluxed for 30 minutes. After cooling, the yield of the elegant reagent benzylmagnesium chloride was measured. 80%, the obtained Grignard reagent does not need to be further processed, and is reserved for subsequent Grignard reactions with other substances.

example 2

[0034] Example 2: The dry four-necked flask was simply evacuated with nitrogen, and then 12 g of fresh Mg, 24 mol of benzyl chloride, and 180 ml of tetrahydrofuran were put into the four-necked flask. Mix evenly, place in an ultrasonic device for ultrasonic reaction, the reaction is initiated within 20 seconds, and the reaction ends after 20 minutes. The reaction is milder than using ether as a solvent, but attention should also be paid to removing part of the reaction heat in time, and the reaction is complete Then reflux for 20 minutes. After cooling, it was determined that the yield of the Grignard reagent benzylmagnesium chloride was 82%, and the obtained Grignard reagent did not need to be further processed, and was left to undergo Grignard reaction with other substances later.

[0035] Example 3: The reaction steps are the same as in Example 2, but start without nitrogen evacuation, and the yield of the Grignard reagent benzylmagnesium chloride obtained by the reaction i...

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Abstract

The present invention discloses phonochemical process of preparing benzyl magnesium chloride as Grignard reagent. The process adopts industrial level tetrahydrofuran or ethyl ether as solvent, and performs ultrasonic reaction in initially nitrogen exhausted reactor with ultrasonic source in reaction initiating time of 10-20 sec and yield of 70-82, without need of special treatment on solvent, continuous nitrogen introduction and initiator. The phonochemical process of preparing benzyl magnesium chloride has mild reaction condition, high yield, low cost, easy industrial application and other features.

Description

technical field [0001] The invention relates to a method for preparing Grignard reagent benzylmagnesium chloride by sonochemical method. Background of the invention [0002] Grignard reagents are of great significance in the pharmaceutical industry, perfume industry, catalysts for polymerization reactions, and the synthesis of other metal organic compounds. [0003] The preparation of Grignard reagent is to use diethyl ether and tetrahydrofuran as solvent, through the reaction of metal magnesium and organic halide, the reaction formula is as follows: [0004] <chemistry num="001"> <chem file="200410051433_cml001.xml" / > < / chemistry> [0005] The main factors affecting the preparation of Grignard reagent are the structure of halogenated hydrocarbon, solvent, purity of magnesium powder, temperature and so on. The traditional process is usually difficult at the beginning of the reaction, and an initiator needs to be added for the reaction to occur. The re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/02
Inventor 邓淑华黄慧民漆小龙周立清吴昭俏
Owner GUANGDONG UNIV OF TECH