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Preparation method of methyl-magnesium chloride

A technology of methylmagnesium chloride and metal magnesium, applied in the direction of magnesium organic compounds, etc., can solve the problems that the application is not widely favored, the price is high, and the cost of methylmagnesium chloride is high.

Active Publication Date: 2009-10-14
HANGZHOU JINFADA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Methyl iodide is expensive and is usually only used in the synthesis of high-value chemicals. Methyl bromide has not been used in synthesis due to disadvantages such as its price, toxicity, and other unfavorable factors such as being a gas at normal temperature. widely favored
[0003] Chloromethane Grignard reagent (methylmagnesium chloride) can be synthesized by conventional methods, that is, anhydrous tetrahydrofuran or anhydrous ether and ethylene glycol dimethyl ether, etc. are used as solvents, and synthesized by methyl chloride and metal magnesium. Solvents such as anhydrous ether and ethylene glycol dimethyl ether are more expensive, and it is more troublesome to recycle and apply mechanically, so the cost of synthetic methylmagnesium chloride is relatively high

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0016] Embodiment 1: feed a small amount of methyl chloride gas in the atmospheric pressure reaction bottle that 2.4g magnesium and 40g pure methylal are housed, after reaction exothermic triggering, feed into methyl chloride gas slowly to magnesium reaction completely again, obtain final product Grignard Reagent - Methyl Magnesium Chloride.

Embodiment 2

[0017] Embodiment 2: 5.1g liquid methyl chloride is added in the autoclave that 2.4g magnesium and 40g pure methylal are housed, and reaction exothermic, appears to descend automatically until the temperature of Grignard reaction, then keep warm and stir for half an hour, obtain formazan Magnesium Chloride.

Embodiment 3

[0018] Example 3: Add 5.5 g of liquid methyl chloride to an autoclave equipped with 2.4 g of magnesium and 30 g of pure methylal, the reaction is exothermic until the temperature of the Grignard reaction drops automatically, and then stirred for half an hour to obtain methyl magnesium chloride.

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PUM

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Abstract

The invention relates to a preparation method of methyl-magnesium chloride, belonging to the technical field of preparation method of Grignard reagent. The method is characterized in that: reaction is implemented by taking methyl chloride and magnesium metal as raw materials and methylal as a solvent, wherein the molar ratio between the magnesium metal and the methyl chloride is 1:0.5 to 3, and the weight ratio between the magnesium metal and the methylal is 1:2 to 100. The method carries out the reaction by taking the methyl chloride and the magnesium metal as raw materials and the methylal as the solvent, thus lowering the production cost; furthermore, the recycling of the methylal is easy, thus further lowering the production cost. The raw material can also be prepared from byproducts of glyphosate production, therefore, the source of raw materials are rich, the cost is low, furthermore, the purification and separation cost of the byproducts is reduced, and the production technology is simple and easy, thus having obvious economic benefit.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of Grignard reagents, in particular to a preparation method of methylmagnesium chloride. Background technique [0002] Grignard reagent is a metal-organic compound with the general formula RMgX (R represents a hydrocarbon group, X represents a halogen). In 1901, F.-A.V. Grignard used halogenated hydrocarbon RX and magnesium to react in ether solution for the first time. As an important methylating reagent, the Grignard reagent of methyl halide has been widely used in the synthesis of drugs, pesticides, flavors and food additives. Methyl iodide is expensive and is usually only used in the synthesis of high-value chemicals. Methyl bromide has not been used in synthesis due to disadvantages such as its price, toxicity, and other unfavorable factors such as being a gas at normal temperature. Widely favored. [0003] Chloromethane Grignard reagent (methylmagnesium chloride) can be synthe...

Claims

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Application Information

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IPC IPC(8): C07F3/02
Inventor 李景华孔鑫明俞叶明刘劭农王伟
Owner HANGZHOU JINFADA CHEM IND
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