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Synthesis process of 2, 3-difluoro-4-alkoxy phenol

A technique for the synthesis of alkoxyphenols, which is applied in the field of synthesis techniques of 2,3-difluoro-4-alkoxyphenols, can solve the problems of difficulty in purifying qualified products, low yields, and poor reaction effects, and achieve The effect of low cost, low equipment requirements and mild reaction conditions

Pending Publication Date: 2020-03-27
BENGBU CHINA SYNCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the first step, the author directly carries out the oxidation reaction without treatment, and needs to add a large amount of formic acid. The reaction effect is poor. and impurities are not introduced in detail

Method used

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  • Synthesis process of 2, 3-difluoro-4-alkoxy phenol
  • Synthesis process of 2, 3-difluoro-4-alkoxy phenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1: 1000mL four-neck bottle, equipped with a thermometer and a condenser tube, under nitrogen protection, put 57.6g (0.4mol) of 2,3-difluoroanisole and 440mL of tetrahydrofuran, start stirring, and cool down to -85°C in a low-temperature bath At ~-75°C, 192 mL (0.48 mol) of n-butyl lithium in n-hexane solution (2.5 mol / L) was slowly added dropwise. After the addition was complete, the mixture was stirred at controlled temperature for 2.0 hours. After the heat preservation is completed, 62.3 g (0.6 mol) of trimethyl borate is started to be added dropwise at a controlled temperature of -85°C to -75°C, and the dropwise addition is completed and the temperature is kept for 2.0 hours. The residual raw material of 2,3-difluoroanisole detected by liquid phase detection in the sample delivery was less than 0.5%.

[0028] After the reaction is complete, negative pressure precipitates tetrahydrofuran until the temperature of the reaction bottle reaches 50°C and there is no fl...

Embodiment 2

[0031] The first step: 1000mL four-neck bottle, equipped with a thermometer and a condenser, under the protection of nitrogen, put 63.3g (0.4mol) of 2,3-difluorophenethyl ether and 480mL of tetrahydrofuran, start stirring, and cool down to -85°C in a low-temperature bath At -75°C, 192 mL (0.48 mol) of n-butyl lithium in n-hexane (2.5 mol / L) was slowly added dropwise, and after the addition was complete, the mixture was stirred under temperature control for 2.0 hours. After the heat preservation is completed, 87.6 g (0.6 mol) of triethyl borate is started to be added dropwise at a controlled temperature of -85°C to -75°C, and the dropwise addition is completed and the temperature is kept for 2.0 hours. The residual raw material of 2,3-difluorophenetole was detected by liquid phase detection <0.5%.

[0032] After the reaction is complete, negative pressure precipitates tetrahydrofuran until the temperature of the reaction bottle reaches 50°C and there is no flow, stop the precip...

Embodiment 3

[0035] The first step: 1000mL four-neck bottle, equipped with a thermometer and a condenser, under the protection of nitrogen, put 63.3g (0.4mol) of 2,3-difluorophenetole and 480mL of tetrahydrofuran, start stirring, and cool down to -70°C in a low-temperature bath At -60°C, 192 mL (0.48 mol) of a cyclohexane solution of n-butyllithium (2.5 mol / L) was slowly added dropwise. After the addition was complete, the mixture was stirred at a controlled temperature for 2.0 hours. After the heat preservation is completed, 112.9 g (0.6 mol) of isopropyl borate is started to be added dropwise at a controlled temperature of -70° C. to -60° C., and the dropwise addition is completed and the temperature is kept for 2.0 hours. The residual raw material of 2,3-difluorophenetole was detected by liquid phase detection in sample delivery <0.5%.

[0036]After the reaction is complete, negative pressure precipitates tetrahydrofuran until the temperature of the reaction bottle reaches 50°C and ther...

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Abstract

The invention discloses a synthesis process of 2, 3-difluoro-4-alkoxy phenol, and belongs to the technical field of organic synthesis. The process comprises the following steps: using 2, 3-difluorophenylalkyl ether as a raw material, carrying out lithiation by use of n-butyllithium under an ultralow temperature condition, reacting with boric acid ester, adding an alkali for quenching to obtain 2,3-difluoro-4-alkoxy benzene borate, oxidizing in the presence of hydrogen peroxide, and performing acidolysis to obtain 2, 3-difluoro-4-alkoxy phenol, so that the purity of the purified product can reach more than 99.95 %, the impurity content is less than 50ppm, and the requirements of electronic-grade products are met. Boric acid and the alkali can form salt, the salt is dissolved in water and subjected to a homogeneous reaction for an oxidation reaction during oxidation in the presence of the hydrogen peroxide, the reaction conditions are mild, impurities are few, the product purity is high, the solvent can be recycled, and industrial production is easy to achieve.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a synthesis process of 2,3-difluoro-4-alkoxyphenol. Background technique [0002] 2,3-difluoro-4-alkoxyphenol is a kind of commonly used fine chemical intermediates. Due to the special properties of fluorine atoms, its single crystal or mixed crystal is widely used in projectors, televisions, mobile phones and other displays. Screen. Therefore, with the development of liquid crystal display technology, the requirements for research and development of new liquid crystal materials are becoming more and more urgent. For the synthesis of 2,3-difluoro-4-alkoxyphenol, the literature reports are as follows: [0003] In US6319570, 2,3-difluorophenetole is used as raw material, and n-butyllithium is added dropwise at -78°C, and then reacted with boric acid ester. The reaction was directly raised to room temperature without any treatment, added formic acid, added dropwise hydr...

Claims

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Application Information

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IPC IPC(8): C07C41/26C07C43/23
CPCC07C41/26C07F5/025C07C43/23
Inventor 徐剑霄刘洪强赵士民魏佳玉王松松朱克明
Owner BENGBU CHINA SYNCHEM TECH CO LTD
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