Preparation method for 2-chloro-6-fluorophenol

A technology of fluorophenol and o-fluorophenol, applied in the field of preparation of 2-chloro-6-fluorophenol, can solve the problems of low reaction temperature, high price, inability to operate and produce in large quantities, etc., and achieves the effects of simple operation and low cost

Inactive Publication Date: 2013-12-11
上海敖合化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] The disadvantages of the above two preparation methods are: due to the extremely low reaction temperature and the need to use expensive, water- and air-sensitive lithium reagents, the above-mentioned methods cannot be industrially produced in large quantities.

Method used

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  • Preparation method for 2-chloro-6-fluorophenol
  • Preparation method for 2-chloro-6-fluorophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] ⑴Add 10mL CH to a 100mL three-necked bottle 2 Cl 2 and 2.0g (0.018mol) o-fluorophenol, slowly drop 20mL (0.032mol) NaClO solution (active chlorine 5.68g / 100mL, 1.6mol / L) into the there-necked flask through the dropping funnel, the color gradually changes during the dropping process Deep; the reaction temperature is kept at about 40°C, and GC tracking is performed every 30 minutes. After 1 hour of reaction, GC tracking confirms that the reaction is terminated; (2) Add 2-6mol / L dilute hydrochloric acid to the three-necked flask to neutralize the reaction, so that the reaction solution becomes weak acidic, adjust the pH to be 6, and stand to separate the organic phase; (3) the organic phase separated in step (2) is washed with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and the solvent is removed by rotary evaporation under reduced pressure to obtain a crude product, and the crude product is then The product 2-chloro-6-fluorophenol was...

Embodiment 2

[0024] In this example, 16 mL of NaClO solution was used in step (1) to replace 20 mL of NaClO solution in step (1) of Example 1, and the remaining operations were the same as in Example 1 to obtain 2.1 g of the product 2-chloro-6-fluorophenol with a yield of 80% , 98.3% purity.

Embodiment 3

[0026] In the present embodiment, use 15mLCCl in step (1) 4 10mLCH in alternative embodiment 1 step (1) 2 Cl 2 , the remaining operations were the same as in Example 1 to obtain 2.0 g of the product 2-chloro-6-fluorophenol, with a yield of 76.5% and a purity of 98%.

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Abstract

The invention discloses a preparation method for 2-chloro-6-fluorophenol. The preparation method comprises the following steps of: (1) adding o-fluorophenol in a reactor, slowly dripping sodium hypochlorite aqueous solution in the reactor, wherein the molar ratio of sodium hypochlorite to o-fluorophenol is (1.0 to 2.0): 1, heating the reactor to 0-77 DEG C, insulating heat and reacting, so as to generate the mixture of 2-chloro-6-fluorophenol; (2) after the reaction is concluded, adding diluted hydrochloric acid in the reactor, adjusting pH value to be 5-6.5, and standing to separate out an organic phase; and (3) purifying and drying the organic phase separated in the step (2) to obtain 2-chloro-6-fluorophenol. The preparation method aforementioned is simple to operate, low in cost, and capable of being industrially operated and produced in large batches.

Description

technical field [0001] The present invention relates to a preparation method of 2-chloro-6-fluorophenol. Background technique [0002] 2-Chloro-6-fluorophenol is an important fluorine-containing fine chemical, as well as an important pharmaceutical and pesticide intermediate. Currently known preparation methods include the following two: [0003] One is to use ortho-fluorophenol as a raw material, amide group protection, selective lithiation at -78°C under harsh anhydrous and oxygen-free low temperature, and then react with 1,2-dichloroethane, with a yield close to 90%. Obtain 2-chloro-6-fluorophenol, the reaction formula is as follows: [0004] [0005] The other is to use m-fluorochlorobenzene as a raw material to obtain 2-chloro-6-fluorophenol with a yield of about 94% through selective lithiation, silicification and oxidation at a harsh anhydrous and oxygen-free low temperature -78°C. The formula is as follows: [0006] [0007] The disadvantages of the above t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/28C07C37/62
Inventor 程经顺倪建彬江维崇杨涛
Owner 上海敖合化工科技有限公司
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