Technical method for synthesizing 4-fluoroaniline by electrochemistry method

A p-fluoroaniline and electrochemical technology, applied in the field of electrochemical synthesis of p-fluoroaniline, can solve the problems of many by-products, difficult separation, complex composition of electrolyte, etc., and achieve the effects of saving consumption and reducing costs

Active Publication Date: 2009-06-17
LAVIANA TAIZHOU PHARMACHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the solubility of p-fluoronitrobenzene in water is low, and additives such as surfactants need to be added to increase its

Method used

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  • Technical method for synthesizing 4-fluoroaniline by electrochemistry method
  • Technical method for synthesizing 4-fluoroaniline by electrochemistry method
  • Technical method for synthesizing 4-fluoroaniline by electrochemistry method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] In a two-chamber electrolytic cell with each chamber being 100mL, the anode chamber is filled with H at a concentration of 30%. 2 SO 4 Solution, 5% p-fluoronitrobenzene, 1-methyl-3-butylimidazolium tetrafluoroborate, and 10% water were added to the cathode chamber. Both anode and cathode are graphite. The cation exchange membrane is PE-100 type cation exchange membrane. Apply direct current between the cathode and anode for electrolysis. After the reaction was completed, the catholyte was extracted with ether to separate aniline. The cathode current efficiency is greater than 90%. The yield of p-fluoroaniline is greater than 98%.

Embodiment 2

[0059] In a two-chamber electrolytic cell with each chamber being 100mL, the anode chamber is filled with H at a concentration of 30%. 2 SO 4 Solution, 5% p-fluoronitrobenzene, 1-methyl-3-ethylimidazolium tetrafluoroborate, and 10% water were added to the cathode chamber. Both anode and cathode are graphite. The cation exchange membrane is PE-100 type cation exchange membrane. Apply direct current between the cathode and anode for electrolysis. After the reaction is finished, the catholyte is extracted with ether to separate aniline. The cathode current efficiency is greater than 90%. The yield of p-fluoroaniline is greater than 98%.

Embodiment 3

[0061] In a two-chamber electrolytic cell with each chamber being 100mL, the anode chamber is filled with H at a concentration of 30%. 2 SO 4 Solution, 5% p-fluoronitrobenzene, 1-methyl-3-butylimidazolium hexafluorophosphate, and 2% water were added to the cathode chamber. Both anode and cathode are graphite. The cation exchange membrane is PE-100 type cation exchange membrane. Apply direct current between the cathode and anode for electrolysis. After the reaction was completed, the catholyte was extracted with ether to separate aniline. The cathode current efficiency is greater than 90%. The yield of p-fluoroaniline is greater than 95%.

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Abstract

The invention relates to a technical method for electrochemically synthesizing para-fluoroaniline. An electrochemical reaction of the invention occurs in a double-chamber diaphragm electrolytic cell, and an anode chamber and a cathode chamber of the electrolytic cell are separated by a cation exchange membrane. An anode is made of such anode materials as graphite, DSA or lead and the like; and a cathode is made of such materials as platinum, silver, copper, lead, nickel, a copper nickel alloy, a copper amalgam alloy, carbon steel, stainless steel, the graphite, glassy carbon and the like. Catholyte consists of 1-20% of nitrobenzene, 1-30% of water and ionic liquid; and anolyte is 5-50% of sulfuric acid or other acidic solution, alkali solutions and salt solutions. An electrolysis product of the cathode is the para-fluoroaniline. The technical method for synthesizing the para-fluoroaniline in the ionic liquid has the advantages of simple process, high yield, little pollution and low cost.

Description

technical field [0001] The invention relates to a technical method for electrochemically synthesizing p-fluoroaniline. Background technique [0002] p-Fluoroaniline is an important intermediate, widely used in the synthesis of new fluorine-containing medicines, pesticides and dyes. The production method of p-fluoroaniline at present has: [0003] 1. One-step method The better process in the one-step method is the nitrobenzene method, which is obtained through deoxidation, hydrogenation and fluorination. with PtO 2 For the catalyst, BF 3 -HF is a fluorinating agent, hydrogen is a reducing agent, and reacted at 42° C. for 12.5 hours, the reaction conversion rate is 100%, and the yield reaches 95%. 2. The two-step method synthesizes p-fluoronitrobenzene from different raw materials, and then reduces and hydrogenates p-fluoroaniline. There are many methods: (1) p-Chloronitrobenzene fluorination method The fluorination catalyst has a styrene copolymer as a substrate, grafted...

Claims

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Application Information

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IPC IPC(8): C25B3/04C07C211/52C25B3/25
Inventor 陈松陈红清杨光陈文霆
Owner LAVIANA TAIZHOU PHARMACHEM
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