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Production method of trifluoromethoxybenzene

A technology of trifluoromethoxybenzene and production method, applied in the production of trifluoromethoxybenzene and the production field of aromatic compounds, can solve the problems of reduced yield, high cost and high consumption, achieve high recovery rate, The effect of smooth response and reduced usage

Active Publication Date: 2016-10-12
SHANDONG DOCRIS CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Find a suitable initiator to reduce the chlorination side reaction on the benzene ring, and find a suitable feeding method to solve the one-time feeding, commonly known as "one-pot cooking" chlorination reaction, the reaction will proceed to the ring chlorination, resulting in a large amount of ring chlorine Chemical by-products, resulting in reduced yield, high consumption, and high cost

Method used

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  • Production method of trifluoromethoxybenzene
  • Production method of trifluoromethoxybenzene

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specific Embodiment approach

[0032] The present invention will be further described below through examples, but the protection scope of the present invention is not limited thereto.

[0033] The raw materials used in this example are all commercially available products. The analysis of the reaction process adopts gas chromatography analysis method.

[0034] The chemical reaction formula of the present embodiment is as follows:

[0035]

Embodiment 1

[0037] 1. Chlorination reaction

[0038]Add 150g of p-chlorobenzotrifluoride solvent into a 1000ml reactor equipped with mechanical stirring, condenser, thermometer, bottom vent pipe, and dropping pipe, start stirring, heat up to 139-140°C, until the solvent refluxes, pass Chlorine gas, start dropwise adding a mixed solution of 200g of anisole, 600g of p-chlorobenzotrifluoride solvent and 10g of azobisisobutyronitrile initiator, and add dropwise at 139-140°C for about 12 hours. After the dropwise addition is completed, take a sample for analysis. When dichloromethoxybenzene is lower than 0.3%, stop the reaction and lower the temperature.

[0039] 2. Fluorination reaction

[0040] Add 1134.5g of the mixed solution obtained from the chlorination reaction into a 1L autoclave, add 133.3g of hydrogen fluoride, start stirring, raise the temperature to 95°C, and keep the reaction under a pressure of 2.8Mpa for 3-4h. Stop the reaction and take a sample for analysis.

[0041] 3. Pro...

Embodiment 2

[0044] 1. Chlorination reaction

[0045] Add 450g of p-chlorobenzotrifluoride solvent into a 3000ml reactor equipped with mechanical stirring, condenser, thermometer, bottom vent tube, and dropping tube, start stirring, and raise the temperature to 139-140 degrees Celsius to reach 450 g of p-chlorobenzotrifluoride solvent. When reflux occurs, pass chlorine gas, and start to drop a mixed solution of 600g of anisole, 1200g of p-chlorobenzotrifluoride solvent and 30g of azobisisobutyronitrile initiator, dropwise at 139-140°C for about 12 hours, dropwise Sampling and analysis after completion, when dichloromethoxybenzene is less than 0.3%, stop the reaction and cool down.

[0046] 2. Fluorination reaction

[0047] Add 2811.91g of the mixed solution obtained from the chlorination reaction into the autoclave, add 400.0g of hydrogen fluoride, start stirring, raise the temperature to 90°C, and keep the reaction under 2.5Mpa pressure for 3-4h. Stop the reaction and take a sample for ...

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Abstract

The invention relates to a production method of an aromatic compound, in particular to a production method of trifluoromethoxybenzene. The production method includes chlorination reaction, fluoridation reaction and product separation and is characterized in that anisole is used as the initial raw material, the chlorination reaction uses aromatic hydrocarbon containing fluorine as the solvent, the solvent cannot be separated after the reaction, the fluoridation reaction of the solvent and HF is performed under proper conditions, the reaction products of the fluoridation reaction are subjected to washing and layering, the lower oil phase is subjected to rectification to obtain the trifluoromethoxybenzene, and the solvent is recycled. The purity of the obtained trifluoromethoxybenzene is larger than 99%, and the yield of the trifluoromethoxybenzene is larger than 95%. The chemical reaction formula is shown as follows.

Description

technical field [0001] The invention belongs to the field of organic synthesis technology, in particular to a production method of aromatic compounds, in particular to a production method of trifluoromethoxybenzene. Background technique [0002] Trifluoromethoxybenzene can be used in pesticides, medicines and liquid crystals. Medicines synthesized with fluorine-containing organic compounds as raw materials have many advantages: as they can enhance the drug properties of medicines, have high curative effect, and have no other side effects, and also have the characteristics of persistence and good oral sex. In recent years, this organic compound has been widely used. [0003] "The Properties, Synthesis and Application of Trifluoromethoxybenzene Derivatives" published by Zhang Chao and Zang You in the 2nd issue of "Organic Fluorine Industry" in 2008 proposed several methods: 1. Using anisole As a substrate, it is obtained by chlorination and fluorination. 2. Using trichlorome...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/22C07C43/225
CPCC07C41/22C07C43/225
Inventor 王德强于文智类成存赵贵敏
Owner SHANDONG DOCRIS CHEM
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