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Synthetic method of octafluorotoluene

A technology of octafluorotoluene and synthesis method, applied in chemical instruments and methods, organic chemistry, preparation of halogenated hydrocarbons, etc., can solve the problems of difficult tar handling, high fluorination temperature, many side reactions, etc., and achieves the production of less tar, Fewer side reactions and the effect of lowering the reaction temperature

Active Publication Date: 2021-03-05
DALIAN QIKAI MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The production of fluorinated toluene in the prior art mostly uses chlorinated toluene as raw material for fluorination, the fluorination temperature of chlorine on the benzene ring is high, there are many side reactions, it is easy to coke, tar is difficult to handle, and environmental protection is under great pressure

Method used

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  • Synthetic method of octafluorotoluene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] First step response:

[0027] Take a 3000mL four-neck flask with stirring, thermometer, and reflux condenser. Add 312g of 98% sulfuric acid, slowly add 72g of water, and lower the temperature to 0-5°C. Add 1000 g of pentafluorobenzene and 357 g of paraformaldehyde. 1160 g of chlorosulfonic acid was added dropwise. After the dropwise addition, the temperature was raised to 45° C., and a sample was taken after reacting for 2 hours. The raw material trifluoromethylbenzene was ≤10%. The temperature is lowered and stratified, the upper layer is the organic phase, and the lower layer is the waste concentrated sulfuric acid. Add 1000 g of water to the upper layer, stir, wash with water, and separate layers.

[0028] The upper layer is the aqueous phase, and the lower layer is the organic phase. Add 5% sodium hydroxide solution to the lower organic phase to adjust the pH to neutral. The layers are separated, and the lower layer is transferred to a still pot for rectificat...

Embodiment 2

[0034] First step response:

[0035] Take a 3000mL four-neck flask with stirring, thermometer, and reflux condenser. Add 312g of 98% sulfuric acid, slowly add 72g of water, and lower the temperature to 0-5°C. Add 1000 g of pentafluorobenzene and 320 g of paraformaldehyde. 1044 g of chlorosulfonic acid was added dropwise. After the dropwise addition, the temperature was raised to 35° C., and a sample was taken after reacting for 2 hours. The raw material trifluoromethylbenzene was ≤10%. Cooling and layering, adding 1000g of water to the upper layer, washing with water, and layering. Add 5% sodium hydroxide solution to the lower organic phase to adjust the pH to neutral. The layers are separated, and the lower layer is transferred to a still pot for rectification. The distillate before rectification is the raw material pentafluorobenzene, which is recovered for the next batch of reactions. At an oil temperature of 150°C, a top temperature of 120°C, and a pressure of -0.085...

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PUM

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Abstract

The invention relates to a synthetic method of octafluorotoluene, belonging to the technical field of fine chemical intermediate synthesis. According to a technical scheme in the invention, the preparation method comprises the following steps: 1) with pentafluorobenzene, paraformaldehyde and chlorosulfonic acid as raw materials, carrying out chloromethylation to obtain an intermediate, namely pentafluorobenzyl chloride; 2) chloridizing the intermediate with chlorine under illumination to obtain an intermediate, namely 1,2,3,4,5-pentafluoro-6-(trichloromethyl)benzene; and 3) with DMF as a solvent, conducting fluorinating with potassium fluoride to obtain the product octafluorotoluene. The method is simple in process, uses easily available raw materials and is easy for industrial production.

Description

technical field [0001] The invention relates to the field of synthesis of fine chemical intermediates, in particular to a synthesis method of octafluorotoluene. Background technique [0002] Perfluorinated compounds are a class of elemental organic compounds in which the hydrogen connected to the carbon atom in the molecule of the organic compound is replaced by fluorine. Compounds in which all the carbon-hydrogen bonds in the molecule are converted into carbon-fluorine bonds are called perfluorinated organic compounds, and those that are partially substituted are called mono- or polyfluorinated organic compounds. Because fluorine is the most electronegative element, polyfluorinated organic compounds have chemical stability, thermal stability, high surface activity and hydrophobic and oleophobic properties, and have broad application prospects in chemical industry, medicine and liquid crystal materials. [0003] At present, in the prior art, the main processes of producing ...

Claims

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Application Information

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IPC IPC(8): C07C25/13C07C17/20
CPCC07C17/20C07C17/26C07C17/14C07C25/13Y02P20/584
Inventor 孙发明张洪学姜殿宝
Owner DALIAN QIKAI MEDICAL TECH
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