Process for 4- amino-3-fluorophenol

A kind of fluorophenol, the technology of the new process is applied in the field of producing 4-amino-3-fluorophenol, and can solve the problems such as incapability of industrialized production, limited, cumbersome handling and the like

Inactive Publication Date: 2008-10-01
SHANDONG UNIV AT WEIHAI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the subsequent processing is cumbersome and limited by...

Method used

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  • Process for 4- amino-3-fluorophenol
  • Process for 4- amino-3-fluorophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 28.2 grams of o-fluoronitrobenzene; 450 milliliters of deionized water; 27 grams of concentrated sulfuric acid; 20 milliliters of ethanol and 0.6 grams of 0.3% Pt / C into the reaction kettle. The kettle was sealed, and hydrogen was passed through the kettle until the pressure in the kettle reached 0.2 MPa to start stirring at a speed of 600 rpm. The temperature is increased to 120°C, the pressure is increased to 0.4 MPa, and the time is measured for 5.5 hours. After turning off the heating, pass water to lower the temperature to 25℃ and open the kettle. Pt / C in the reaction liquid is removed (recovered by filtration). The reaction liquid is obtained.

[0013] The reaction solution was extracted twice with 100 ml AcOEt, and the organic phase obtained by combining the two times was distilled under reduced pressure to obtain 1.2 g of unreacted raw material. The water phase was put into a 1000ml reaction flask and 200ml AcOEt was added. The pH was adjusted by adding alkali t...

Embodiment 2

[0018] Except that 20 ml of methanol and 0.6 g of 0.3% Pd / C are used, other conditions are the same as in Example 1. The result shows that the HPLC purity is 94%, and the yield is 61%.

Embodiment 3

[0020] Except that the reaction temperature is 30°C, other conditions are the same as in Example 1. The result shows that the conversion rate is low, HPLC purity: 65%, yield: 38%

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Abstract

The invention relates to a new process for producing 4-amino-3-fluorophenol, which takes o-fluoronitrolbenzene as raw material and platinum-carbon or palladium-charcoal as a catalyst and adopts hydrogen pressure reaction to produce the 4-amino-3-fluorophenol in an acidic aqueous solution which contains organic solvents. The production technology is simpler, the production cost is more reasonable and the method is more suitable for industrial production.

Description

Technical field [0001] The invention relates to a new process for producing 4-amino-3-fluorophenol. Background technique [0002] 4-Amino-3-fluorophenol has a wide range of uses. It is an intermediate for pesticides sulfluron, benzopyrrolidone herbicides, phenoxymethyl acetate herbicides, fungicides, hair dyes, etc. There are few reports on the process of 4-amino-3-fluorophenol at home and abroad. The U.S. Patent (US5545754) discloses that o-fluoronitrobenzene is used as a raw material, in an acidic organic solvent aqueous solution, hydrogen is pressurized to react, catalyzed by a catalyst Production of 4-amino-3-fluorophenol. However, the subsequent processing is cumbersome and is limited by the porous extractor, making it impossible for industrial production. Summary of the invention [0003] The present invention aims to provide a new process for producing 4-amino-3-fluorophenol, which is used to overcome the defects of the above-mentioned existing preparation methods. The te...

Claims

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Application Information

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IPC IPC(8): C07C215/76C07C213/00B01J23/40
Inventor 孙德群安永生杨越
Owner SHANDONG UNIV AT WEIHAI
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