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Preparation method of pentafluorophenol

A technology of pentafluorophenol and hexafluorobenzene, applied in the field of preparation of pentafluorophenol, can solve the problems of harsh reaction conditions, difficult catalyst preparation and high cost, and achieve the effects of less side reactions, low cost and less pollution

Active Publication Date: 2019-02-22
DALIAN QIKAI MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as the method announced in Chinese patent CN105384603A, 107011126A, with halogenated fluorobenzene or hexafluorobenzene as raw material, through catalyst catalytic hydrolysis in water or polar organic solvent and water mixed solvent to prepare pentafluorophenol, the method mainly There are disadvantages of harsh reaction conditions, high cost and difficult catalyst preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 75g of hexafluorobenzene, 50g of sodium hydroxide and 100g of water were successively added into a 300ml autoclave. Seal it, heat it to 120-125°C under stirring and keep it warm for 25 hours, cool it down, transfer the reaction system to a 1000ml four-necked flask equipped with a steam distillation device, and add hydrochloric acid dropwise until the pH value is 3. Raise the temperature to 117-127°C to start steam distillation and continuously separate the lower distillate, and stop when the distillate is not separated. Use a 100cm packed rectification column to carry out vacuum rectification on the above receiver with a vacuum degree of 5mmHg, while receiving the fraction at 67-70°C. A product with a purity of over 99% can be obtained with a yield of 95%.

Embodiment 2

[0027] 75g of hexafluorobenzene, 90g of potassium hydroxide and 120g of water were successively added into a 300ml autoclave. Seal it, heat it to 110-115°C under stirring and keep it warm for 40 hours, cool it down, transfer the reaction system to a 1000ml four-necked flask equipped with a steam distillation device, and add hydrochloric acid dropwise until the pH value is 3. Raise the temperature to 117-127°C to start steam distillation and continuously separate the lower distillate, and stop when the distillate is not separated. Use a 100cm packed rectification column to carry out vacuum rectification on the above receiver with a vacuum degree of 5mmHg, while receiving the fraction at 67-70°C. A product with a purity of over 99% can be obtained with a yield of 92%.

Embodiment 3

[0029] 75g of hexafluorobenzene, 60g of sodium hydroxide and 100g of water were successively added into a 300ml autoclave. Seal it, heat it to 120-125°C under stirring and keep it warm for 25 hours, cool it down, transfer the reaction system to a 1000ml four-necked bottle, and add hydrochloric acid dropwise until the pH value is 3. The neutralized reaction system was extracted three times with toluene 200g / time, and the extracts were combined. A 100cm packed rectification column is used to carry out atmospheric rectification on the above-mentioned combined liquid, while receiving the fraction at 142-145°C. A product with a purity of over 99% can be obtained with a yield of 89%.

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Abstract

The invention relates to a preparation method of pentafluorophenol, and belongs to the field of chemical production technologiesprocesses. The preparation method of the pentafluorophenol is carried out according to the following technologies processes that hexafluorobenzene, strong base and water are put in a sealed container, to be prepared intothus a mixed solution is prepared, heat preservationis conducted at the temperature of 100-150 DEG C for reaction, and thus a system solution is obtained; the system solution is neutralized until the pH value is not higher than 6, then a coarse product is extracted, rectification is conducted, and the pentafluorophenol is obtained. According to the preparation method, the cost is low, organic matter and heavy metal are not adopted except for substrate, pollution is small, side reactions is are lessfewer, the reaction steps are simple, and operation is easy.

Description

technical field [0001] The invention relates to a preparation method of pentafluorophenol, which belongs to the field of chemical production technology. Background technique [0002] Pentafluorophenol is an important pharmaceutical intermediate and is mostly used to prepare pentafluorophenyl active esters for peptide synthesis, thereby promoting the formation of peptide bonds. In addition, it is also an important liquid crystal material intermediate, which is suitable for the preparation of polyfluorine monomer liquid crystal materials. [0003] So far, the synthesis methods of pentafluorophenol mainly include: 1. Diazotization hydrolysis. As described in the Chinese patent ZL200510049766.X, bromobenzene is used as a raw material to produce fluorophenol through three steps of ammonification, diazotization and hydrolysis. The limitation of this process is that there are many reaction steps and a large amount of waste water is generated and the pollution is serious. , the by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/27C07C37/02C07C37/76
CPCC07C37/02C07C37/76C07C39/27
Inventor 田瀚卿姜殿平张洪学
Owner DALIAN QIKAI MEDICAL TECH
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