Preparation method of (trifluoromethoxy)benzene compound

A technology of trifluoromethoxybenzene and trichloromethoxybenzene, applied in the field of organic chemical industry synthesis, can solve problems such as solvent consumption, solvent cost and the like

Pending Publication Date: 2021-03-19
KINGCHEM LIAONING CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The common feature of the above-mentioned technologies is that a pure organic compound solvent is used to carry...

Method used

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  • Preparation method of (trifluoromethoxy)benzene compound
  • Preparation method of (trifluoromethoxy)benzene compound
  • Preparation method of (trifluoromethoxy)benzene compound

Examples

Experimental program
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Effect test

Embodiment 1

[0062] With 450g of fluorinated material rectification raffinate (main components: 4-chloro-trifluoromethoxybenzene 35.1%, difluoro-chloromethoxybenzene 20.4%, 4-chloro-difluoro-chloromethoxybenzene 15.7% %), 2.5g of phosphorus trichloride were added into a 1000mL reaction flask equipped with stirring, reflux condenser and chlorine pipe, and the temperature was raised to 120-130°C. Add 150g of anisole and 2.5g of AIBN, and at the same time feed chlorine gas to control the flow rate of chlorine gas to 40-50L / h. The reaction tail gas absorbs HCl therein through water, and then absorbs unreacted chlorine gas with 30% NaOH. After the anisole has been added, continue to feed chlorine, and add a mixed solution of 100g of fluorinated material rectification raffinate and 2g of AIBN. To the content of dichloromethoxybenzene in the reaction solution 2 Purging, precipitation, until the temperature of the kettle is 150°C / -0.096Mpa, the extracted solvent can continue to be used for the ch...

Embodiment 2

[0065] With 450g of fluorinated material rectification raffinate (main components: 20.2% of 4-chloro-trifluoromethoxybenzene, 35.8% of difluorochloromethoxybenzene, 16.7% of 4-chloro-difluorochloromethoxybenzene %), 2.5g of phosphorus trichloride were added into a 1000mL reaction flask equipped with stirring, reflux condenser and chlorine pipe, and the temperature was raised to 120-130°C. Add 150g of anisole and 2.5g of AIBN, and at the same time feed chlorine gas to control the flow rate of chlorine gas to 40-50L / h. The reaction tail gas absorbs HCl therein through water, and then absorbs unreacted chlorine gas with 30% NaOH. After the anisole has been added, continue to feed chlorine, and add a mixed solution of 100g of fluorinated material rectification raffinate and 2g of AIBN. To the content of dichloromethoxybenzene in the reaction solution 2 Purging, precipitation, until the temperature of the kettle is 150°C / -0.096Mpa, the extracted solvent can continue to be used for...

Embodiment 3

[0067] Add 600g of rectification raffinate of fluorinated materials (main components: 41% of 4-chloro-trifluoromethoxybenzene, 35% of 4-chloro-difluoro-chloromethoxybenzene) and 2.5g of phosphorus trichloride to 1000mL In a reaction flask equipped with stirring, a reflux condenser, and a chlorine pipe, the temperature is raised to 120-130°C. Add 200g of 4-chloroanisole and 2.5g of AIBN, and at the same time feed chlorine gas to control the flow rate of chlorine gas to 40-50L / h. The reaction tail gas absorbs HCl therein through water, and then absorbs unreacted chlorine gas with 30% NaOH. After adding 4-chloroanisole, continue to pass chlorine, and add the mixed solution of 100g rectification raffinate of fluorinated material and 2g AIBN. To the content of 4-chloro-dichloromethoxybenzene in the reaction solution 2 Purging, precipitation, until the temperature of the kettle is 150°C / -0.096Mpa, the extracted solvent can continue to be used for the chlorination reaction of 4-chlo...

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Abstract

The invention discloses a preparation method of a (trichloromethoxy)benzene compound and a preparation method of a (trifluoromethoxy)benzene compound. According to the method of the (trichloromethoxy)benzene compound, the (trichloromethoxy)benzene compound is synthesized by taking rectification raffinate, which is generated when a (trifluoromethoxy)benzene compound product is synthesized from the(trichloromethoxy)benzene compound, as a solvent, and the content of the (trichloromethoxy)benzene compound in obtained chlorination liquid can reach 95% or above; and desolventizing is conducted so as to obtain a crude (trichloromethoxy)benzene compound product which can be directly used for a fluorination reaction so as to produce a corresponding (trifluoromethoxy)benzene compound. By utilizingthe method, the waste fluorinated rectification raffinate in the original process can be fully utilized, and waste discharge and treatment cost in the production process are greatly reduced; and sincethe rectification raffinate treated as waste becomes an excellent chlorination reaction solvent, the consumption of raw materials and the production cost are greatly reduced, the purpose of waste utilization is achieved, and a technical process is greener and more environment-friendly.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for preparing trichloromethoxybenzene compounds and a method for preparing trifluoromethoxybenzene compounds based thereon. Background technique [0002] Trifluoromethoxybenzene compounds are a class of important organic synthesis intermediates, among which trifluoromethoxybenzene is widely used in the synthesis of medicines, pesticides, dyes and other products. Trichloromethoxybenzene is an important raw material for the production of trifluoromethoxybenzene. In the prior art, the synthetic method of trifluoromethoxybenzene mainly is, in solvent, in the presence of initiator and light, anisole is chlorinated with chlorine to obtain corresponding trichloromethoxybenzene, and then the trichloromethoxybenzene Methoxybenzene is then fluorinated with HF to obtain trifluoromethoxybenzene. The solvents used for the chlorination of anisole include carbon te...

Claims

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Application Information

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IPC IPC(8): C07C41/22C07C41/42C07C43/225
CPCC07C41/22C07C41/42C07C43/225
Inventor 王富民刘占龙贾铁成王建胡珍珠杨阳
Owner KINGCHEM LIAONING CHEMICAL CO LTD
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