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Synthesis method of 4-bromo-3-methyl anisole

A technology of methyl anisole and synthesis method, applied in chemical instruments and methods, ether preparation, ether separation/purification and other directions, can solve the problem that the quality requirements of downstream products cannot be met, the product purity is only 94%, and the polybromine content Advanced problems, to achieve the effect of safe and friendly production environment, high product purity and high yield

Pending Publication Date: 2022-07-12
SHANDONG MORIS TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the product prepared by the traditional process, the content of polybromine is 2-3%, and the product purity is only 94%
Moreover, the traditional process not only has a long reaction time, resulting in excessive energy consumption, but also uses the volatile solvent hydrogen bromide, which brings environmental pollution, and the product has a high content of polybromine, which makes it unable to meet the quality requirements of synthetic downstream products.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Weigh 1-butyl-3-methylimidazolium bromide and water, mix and stir evenly, and the mass percentage of the ionic liquid solution is 25%;

[0022] (2) Add dropwise bromine to the ionic liquid solution, and stir for 28 minutes after the dropwise addition to obtain an ionic liquid mixed solution; the concentration of bromine in the ionic liquid mixed solution is 18%;

[0023] (3) Weigh m-methyl anisole, at a temperature of 0 °C, according to the molar ratio of bromine and m-methyl anisole of 1:1.1, dropwise add the ionic liquid mixed solution; the dropping time is 40min ;

[0024] (4) After the dropwise addition is completed, continue to stir for 60min, add sodium sulfite solution of decolorizing agent 20wt% according to the molar ratio to the bromine of 1:10 for decolorization, then add deionized water for washing, stir for 25min and then stand for stratification. , remove the lower layer and carry out rectification and purification to obtain the 4-bromo-3-methylanisol...

Embodiment 2

[0026] (1) Weigh 1-ethyl-3-methylimidazolium bromide and water, mix and stir evenly, and the mass percentage of the ionic liquid solution is 30%;

[0027] (2) Add dropwise bromine to the ionic liquid solution, and stir for 32 minutes after the dropwise addition to obtain an ionic liquid mixed solution; the concentration of bromine in the ionic liquid mixed solution is 22%;

[0028] (3) Weigh m-methyl anisole, at a temperature of -2 °C, according to the molar ratio of bromine and m-methyl anisole of 1:1, drop the ionic liquid mixed solution; the dropping time is: 45min;

[0029] (4) After the dropwise addition is completed, continue stirring for 55min, add sodium sulfite solution of 20wt% decolorizer according to the molar ratio to the bromine as 2:10 for decolorization, then add deionized water for washing, stir for 25min and then stand for stratification. , remove the lower layer and carry out rectification and purification to obtain the 4-bromo-3-methylanisole.

Embodiment 3

[0031] (1) Weigh 1-dodecyl-3-methylimidazolium bromide and water, mix and stir evenly, and the mass percentage of the ionic liquid solution is 26%;

[0032] (2) Add dropwise bromine to the ionic liquid solution, and stir for 30 minutes after the dropwise addition to obtain an ionic liquid mixed solution; the concentration of bromine in the ionic liquid mixed solution is 20%;

[0033] (3) Weigh m-methyl anisole, at a temperature of 5 °C, according to the molar ratio of bromine and m-methyl anisole of 1.2:1, drop the ionic liquid mixed solution; the dropping time is 40min ;

[0034] (4) After the dropwise addition is completed, continue stirring for 60min, add the decolorizing agent thiourea dioxide to decolorize according to the molar ratio to the bromine as 2:10, then add deionized water for washing, stir for 30min, let stand for stratification, and remove the lower layer. Carry out rectification and purification to obtain the 4-bromo-3-methylanisole, and the upper layer ioni...

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PUM

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Abstract

The invention discloses a synthesis method of 4-bromo-3-methyl anisole, which comprises the following steps: (1) weighing ionic liquid and water, and uniformly mixing and stirring; (2) dropwise adding bromine into the ionic liquid in the step (1), and stirring for 25-35 minutes after dropwise adding to obtain an ionic liquid mixed solution; (3) weighing m-methyl anisole, and dropwise adding the ionic liquid mixed solution at the temperature of-5 to 10 DEG C according to the molar ratio of bromine to m-methyl anisole being (1: 1)-(1.3: 1); the dropwise adding time is 30 to 60 minutes; and (4) after finishing dropwise adding, continuously stirring for 50-80 minutes, adding a decolorizing agent for decolorizing, adding deionized water for washing, stirring for 20-30 minutes, standing for layering, taking the lower layer, and rectifying and purifying to obtain the 4-bromo-3-methyl anisole. The method is safe and friendly in production environment, low in production energy consumption and production cost, high in conversion rate, high in yield and high in product purity.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a synthesis technology of 4-bromo-3-methylanisole. Background technique [0002] The traditional method for synthesizing 4-bromo-3-methyl anisole is to mix bromine into hydrobromic acid, reduce the temperature of m-methyl anisole to below 5°C, and start adding bromine and hydrobromic acid dropwise. the mixture, control the reaction temperature not higher than 10 ℃, and keep the temperature until the product components are qualified. In the product prepared by the traditional process, the polybromine content is 2-3%, and the product purity is only 94%. Moreover, the traditional process not only has a long reaction time, resulting in excessive energy consumption, but also uses a volatile solvent, hydrogen bromide, which brings environmental pollution, and the polybromine content in the product is high, resulting in the inability to meet the quality requirements of synthe...

Claims

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Application Information

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IPC IPC(8): C07C41/22C07C41/38C07C41/36C07C43/225
CPCC07C41/22C07C41/38C07C41/36C07C43/225Y02P20/54
Inventor 王德强类成存崔淑娜赵晓辉黄伟刘凯
Owner SHANDONG MORIS TECH
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