Method for preparing 2, 3-dimethyl thioanisole

A technology of dimethyl anisole and dimethyl disulfide, which is applied in the field of fine chemical intermediate synthesis, can solve the problems of cumbersome post-processing, high consumption and high cost, avoid post-processing steps, simplify processes, Easy-to-use effects

Active Publication Date: 2021-04-23
JIANGXI TIANYU CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology produces an intermediate product with improved yields but also contains more impurities like didemetoxyfen (DDM) or trimethoate (2,3). These contaminants are difficult to remove from this material due to their low solubility in water making them hard to separate effectively without complicated treatment processes that may be necessary after use.

Problems solved by technology

This patents describes different methods or techniques that have been developed over recent years to improve the efficiency and quality of producing certain compounds called 2, 3 -dim ethyltriazabicyclo heptane (also known as dizoxiboron), which plays key roles in various fields such as pharmaceuticals and agricultural chemistry. These technical problem addressed include improving the efficient manufacturing processes involved in these molecules while reducing costs associated with their use on scales upward.

Method used

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  • Method for preparing 2, 3-dimethyl thioanisole
  • Method for preparing 2, 3-dimethyl thioanisole
  • Method for preparing 2, 3-dimethyl thioanisole

Examples

Experimental program
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Effect test

Embodiment 1

[0037] In a 250mL four-necked flask, add 2.57g (0.04mol, 99.5%) copper powder, 0.5g tetrabutylammonium bromide (TBAB), 56.97g (0.6mol, 99%) dimethyl disulfide , stirred, and the reaction temperature was controlled to be 20°C, and 17.35g (0.16mol, 95%) of tert-butyl nitrite was added dropwise for 0.5 hours. , 99%) 2,3-dimethylaniline, the dropping time is 1.5 hours, after the dropping, the temperature is raised to 50°C, reacted for 4 hours, sampling is carried out in the gas chromatography, and the content of 2,3-dimethylaniline is less than 0.2 %, stop the reaction. The reaction process can be represented by the following reaction equation:

[0038]

[0039] The reaction material was cooled to 25°C, filtered, and the residue was washed twice with dimethyl disulfide, and the amount of dimethyl disulfide was 10 g each time. The organic phases were combined and desolvated under reduced pressure at a vacuum of 4KPa. 15.69 g of crude product was obtained, the quantitative cont...

Embodiment 2

[0041]In a 250mL four-necked bottle, add 6.43g (0.1mol, 99.5%) copper powder, 0.12g tetrabutylammonium chloride (Tetrabutylammonium chloride, TBAC), 23.74g (0.25mol, 99%) dimethyl disulfide , stirred, and the reaction temperature was controlled to be 30°C, and 21.68g (0.2mol, 95%) of n-butyl nitrite was added dropwise for 0.5 hours. After the addition, the temperature was raised to 60°C, 12.22g (0.10mol , 99%) 2,3-dimethylaniline, the dropping time is 0.5 hours, after the drop is completed, the temperature is raised to 75 ° C, and the reaction is carried out for 2 hours, and the sample is controlled by gas chromatography, and the content of 2,3-dimethylaniline is less than 0.2 %, stop the reaction. The reaction process can be represented by the following reaction equation:

[0042]

[0043] The reaction material was cooled to 25°C, filtered, and the residue was washed twice with dimethyl disulfide, and the amount of dimethyl disulfide was 10 g each time. The organic phases...

Embodiment 3

[0045] In a 250mL four-necked bottle, add 0.64g (0.01mol, 99.5%) copper powder, 0.12g tetrabutylammonium iodide (Tetrabutylammonium iodide), 23.74g (0.25mol, 99%) dimethyl disulfide, stir , control the reaction temperature to be 10°C, add 13.01g (0.12mol, 95%) of n-butyl nitrite dropwise, the time for adding is 1.5 hours, after the addition, the temperature is raised to 40°C, and 12.22g (0.10mol, 99% %) 2,3-dimethylaniline, the dropping time is 1.5 hours, after the dropping is completed, the temperature is raised to 50°C, and the reaction is carried out for 4 hours, the sample is controlled by gas chromatography, the content of 2,3-dimethylaniline is less than 0.2%, Stop responding. The reaction process can be represented by the following reaction equation:

[0046]

[0047] The reaction material was cooled to 25°C, filtered, and the residue was washed twice with dimethyl disulfide, and the amount of dimethyl disulfide was 10 g each time. The organic phases were combined a...

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Abstract

The invention provides a method for preparing 2, 3-dimethyl thioanisole, and the method comprises the following step of: reacting 2, 3-dimethyl aniline, alkyl nitrite and dimethyl disulfide serving as raw materials under the catalysis of copper powder and a quaternary ammonium salt to obtain the 2, 3-dimethyl thioanisole. According to the method, the copper powder and the quaternary ammonium salt are used as the catalyst, so that the yield and the purity of the product 2, 3-dimethyl thioanisole are improved, the problems of low yield and low purity of the 2, 3-dimethyl thioanisole in the prior art are solved, the use amount of the copper powder and the dimethyl disulfide in the industrial production process is reduced, and the production cost is reduced. The preparation method provided by the invention is simple, mild in reaction condition and relatively low in production cost, can be used for acquiring 2, 3-dimethyl thioanisole with purity of more than 95%, and is easy for industrial production.

Description

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Claims

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Application Information

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Owner JIANGXI TIANYU CHEM CO LTD
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