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Preparation method of 4-chlorine-3-fluorine benzene ether

A technology of fluorophenetole and fluorophenol, which is applied in the field of preparation of 4-chloro-3-fluorophenetole, can solve the problems of low reaction rate, difficulty in realizing continuous production, troublesome operation, etc., and achieve high reaction rate and short reaction time Shorten and realize the effect of continuity

Inactive Publication Date: 2018-02-23
DONGGUAN LIANZHOU INTPROP OPERATION MANAGEMENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method is cumbersome to operate, it is difficult to realize continuous production, and the reaction rate is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of 4-chloro-3 fluorophenetole, comprising the following steps:

[0025] (1) After mixing deionized water and absolute ethanol, add concentrated sulfuric acid dropwise, and finally add o-fluoronitrobenzene and catalyst into the reactor, seal the reactor, and feed hydrogen into the reactor until the pressure of the reactor is 0.1-0.4 MPa, then stir at 1000 rev / min, while raising the temperature to 60°C, and increase the pressure in the reactor to 0.4-0.6MPa, react for 1h, after the reaction, cool to room temperature, filter, and the obtained filtrate is acetic acid Extracted three times with ethyl ester, collected the organic phase obtained by three extractions, and distilled under reduced pressure to obtain the crude product, then recrystallized and dried the crude product with petroleum ether to obtain 4-amino-3-fluorophenol; 4-amino-3-fluorophenol The purity of the product is 95.68%, and the productive rate is 80.3%; wherein, the catalyst is a pall...

Embodiment 2

[0030] A preparation method of 4-chloro-3-fluorophenetole, comprising the following steps:

[0031] (1) After mixing deionized water and absolute ethanol, add concentrated sulfuric acid dropwise, and finally add o-fluoronitrobenzene and catalyst into the reactor, seal the reactor, and feed hydrogen into the reactor until the pressure of the reactor is 0.1-0.4 MPa, then stirred at 1000 rpm, while raising the temperature to 130°C, and increasing the pressure in the reactor to 0.4-0.6MPa, reacted for 6h, after the reaction, cooled to room temperature, filtered, and the obtained filtrate was filtered with acetic acid Extracted three times with ethyl ester, collected the organic phase obtained by three extractions, and distilled under reduced pressure to obtain the crude product, then recrystallized and dried the crude product with petroleum ether to obtain 4-amino-3-fluorophenol; 4-amino-3-fluorophenol The purity of the product is 99.5%, and the yield is 83.6%; wherein, the cataly...

Embodiment 3

[0036] A preparation method of 4-chloro-3-fluorophenetole, comprising the following steps:

[0037] (1) After mixing deionized water and absolute ethanol, add concentrated sulfuric acid dropwise, and finally add o-fluoronitrobenzene and catalyst into the reactor, seal the reactor, and feed hydrogen into the reactor until the pressure of the reactor is 0.1-0.4 MPa, then stirred at 1000 rev / min, while raising the temperature to 70°C, and increasing the pressure in the reactor to 0.4-0.6MPa, reacted for 2h, after the reaction, cooled to room temperature, filtered, and the obtained filtrate was treated with acetic acid Extracted three times with ethyl ester, collected the organic phase obtained by three extractions, and distilled under reduced pressure to obtain the crude product, then recrystallized and dried the crude product with petroleum ether to obtain 4-amino-3-fluorophenol; 4-amino-3-fluorophenol The purity of the product is 99.99%, and the yield is 90.8%; wherein, the cat...

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PUM

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Abstract

The invention discloses a preparation method of 4-chlorine-3-fluorine benzene ether. The preparation method comprises the following steps: firstly, by taking o-fluoronitrobenzene as a raw material, preparing 4-amino-3-fluorophenol; taking N,N-dimethylformamide as a reaction medium, carrying out acylating chlorination reaction between the 4-amino-3-fluorophenol and an acyl chloride reagent, thus preparing 4-chlorine-3-fluorophenol, mixing sodium phenoxide with a sodium hydroxide aqueous solution, then adding the 4-chlorine-3-fluorophenol, and uniformly stirring and mixing, thus preparing a mixed solution; adding the prepared mixed solution into a reactor, then adding diethyl sulfate, stirring for 3 min, and heating to 80 to 120 DEG C for reaction; at the end of reaction, adjusting the pH ofa reaction system to 2 to 5, allowing the reaction system to stand still for layering, collecting an oil phase, washing the oil phase with the sodium hydroxide aqueous solution, and collecting the oil phase, namely the 4-chlorine-3-fluorine benzene ether. The method disclosed by the invention is easy to operate, low in cost, high in target product purity and high in yield.

Description

Technical field: [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of 4-chloro-3-fluorophenetole. Background technique: [0002] 4-Chloro-3-fluoroanisole is an important pharmaceutical intermediate, which is usually prepared by reacting phenol and alkyl sulfate under alkaline conditions, but the commonly used method is to slowly react at low temperature. The system is carried out by adding the reactants dropwise. However, this method is cumbersome to operate, difficult to realize continuous production, and the reaction rate is low. In order to solve this technical problem, the present invention first prepares 4-chloro-3-fluorophenol with o-fluoronitrobenzene as raw material, then mixes it with a strong alkaline solution containing a small amount of phenoxide, and adds diethyl sulfate to react to prepare The target product has a fast reaction rate and is easy to operate. Invention content: [0003] The object of the pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/225C07C41/16C07C213/00C07C215/76C07C37/00C07C39/27
CPCC07C41/16C07C37/00C07C213/00C07C215/76C07C39/27C07C43/225
Inventor 陈东进
Owner DONGGUAN LIANZHOU INTPROP OPERATION MANAGEMENT CO LTD
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