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The preparation method of 2-chloro-4'-fluoroacetophenone

A technology of fluoroacetophenone and chlorination, which is applied in the field of preparation of 2-chloro-4'-fluoroacetophenone, which can solve the problem of high energy consumption, product irritation and safety, high environmental risk, and a large amount of aluminum trichloride Organic waste liquid and other problems, to achieve the effect of mild reaction conditions, green reaction, cost reduction and solid waste generation

Active Publication Date: 2020-12-22
LIER CHEM CO LTD
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Problems solved by technology

[0004] The technical problem to be solved by the present invention is that the energy consumption of the existing method is relatively high, a large amount of waste water and organic waste liquid containing aluminum trichloride will be produced, and the product has a strong irritant, resulting in high safety and environmental risks.

Method used

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  • The preparation method of 2-chloro-4'-fluoroacetophenone
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  • The preparation method of 2-chloro-4'-fluoroacetophenone

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preparation example Construction

[0016] The preparation method of 2-chloro-4'-fluoroacetophenone comprises the following steps:

[0017] a. Add chloroacetyl chloride dropwise to fluorobenzene and ionic liquid at 0-30°C, and continue to react at 0-30°C after the addition is completed;

[0018] b. After the reaction is complete, distill to obtain 2-chloro-4'-fluoroacetophenone.

[0019] In the above-mentioned preparation method of 2-chloro-4'-fluoroacetophenone, the ionic liquid described in step a is an aluminum chloride-type ionic liquid. Described aluminum chloride type ionic liquid is [emim]Cl-0.5AlCl 3 、[emim]Cl-0.67AlCl 3 、[emim]Cl-0.75AlCl 3 、[emim]Cl-0.8AlCl 3 、[bmim]Cl-0.5AlCl 3 、[bmim]Cl-0.67AlCl 3 、[bmim]Cl-0.75AlCl 3 、[bmim]Cl-0.8AlCl 3 、[mmim]Cl-0.67AlCl 3 、[pmim]Cl-0.67AlCl 3 、[beim]Cl-0.67AlCl 3 , [veim]Cl-0.67AlCl 3 , [eim]Cl-0.67AlCl 3 、[amim]Cl-0.67AlCl 3 、[emmim]Cl-0.67AlCl 3 , [mim]Cl-0.67AlCl 3 or [eeim]Cl-0.67AlCl 3 any of the.

[0020] In the above preparation method of ...

Embodiment 1

[0028] Add 97g (1.01mol, 1.01eq) of fluorobenzene and 206.6g (0.5mol, 0.5eq) of ionic liquid [emim]Cl-0.67AlCl into a 500mL reaction flask 3 113 g (1 mol, 1 eq) of chloroacetyl chloride was added dropwise at room temperature, and stirring was continued for 30 minutes after the addition was completed. The central control fluorophenyl basically disappeared, and then the reaction solution was distilled under reduced pressure under a pressure of 10mmHg, and the fractions at 128°C to 132°C were collected to obtain 169.3g of 2-chloro-4'-fluoroacetophenone. The selectivity of the reaction 99.5%, content 99.5%, yield 98.1%.

Embodiment 2

[0030] Add 98g (1.02mol, 1.02eq) of fluorobenzene and 220.7g (0.5mol, 0.5eq) of ionic liquid [bmim]Cl-0.67AlCl into a 500mL reaction flask 3 , 113 g (1 mol, 1 eq) of chloroacetyl chloride was added dropwise at 0° C., and the stirring reaction was continued for 1.5 hours after the dropwise addition was completed. The central control fluorophenyl basically disappeared, the temperature was raised to 130°C, and 167.2g of 2-chloro-4'-fluoroacetophenone was obtained by distillation under reduced pressure under the condition of 10mmHg, the content was 99.2%, and the yield was 96.87%.

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Abstract

The invention belongs to the field of organic synthesis and particularly relates to a preparation method of 2-chloro-4'-fluoroacetophenone. The technical problems to be solved by the invention are that in the prior art, the energy consumption is higher, a large amount of aluminum chloride wastewater and organic waste liquor can be generated, and raw materials have strong irritation. The scheme of solving the technical problems is to provide the preparation method of the 2-chloro-4'-fluoroacetophenone; the preparation method comprises the following steps: a, dropwise adding chloroacetyl chloride into fluorobenzene and ionic liquid under the condition of room temperature; b, reacting for 20-50 minutes at a normal temperature after the completion of dropwise adding and distilling to obtain the 2-chloro-4'-fluoroacetophenone. The method provided by the invention has the advantages of being simple in operation process and easy for industrialization realization.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of 2-chloro-4'-fluoroacetophenone. Background technique [0002] 2-Chloro-4'-fluoroacetophenone is an important fine chemical intermediate, which can be used to synthesize the medicine fluvastatin and the pesticide epoxiconazole, etc. [0003] The traditional method for synthesizing 2-chloro-4'-fluoroacetophenone is to prepare it by Friedel-Crafts reaction with fluorobenzene and chloroacetyl chloride under the catalysis of anhydrous aluminum trichloride. The reaction is generally carried out in an organic solvent such as a large excess of fluorobenzene or dichloroethane, and the reaction usually needs to be carried out at a low temperature. The reaction time is generally 1 to 2 hours. After the reaction is completed, concentrated hydrochloric acid needs to be added for acidolysis. In order to obtain the final target product. The disadvantage of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/80C07C45/46
CPCC07C45/46C07C49/80
Inventor 李世洪程柯王福雄
Owner LIER CHEM CO LTD
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