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Synthesis method of 2,4-dichloro-5-fluorobenzoyl chloride

A technology of fluorobenzoyl chloride and synthesis method, which is applied in the synthesis field of 2,4-dichloro-5-fluorobenzoyl chloride, can solve the problems of low yield, reduced production efficiency, high price and the like, and achieves broad application prospects , The effect of solving the production cost and simplifying the production process

Active Publication Date: 2015-12-23
SHANDONG GUOBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the prior art, the second step reaction mostly uses FeCl 3 Catalytic hydrolysis, yield up to 99.5%, but FeCl 3 Immediately inactivate after the catalytic reaction, the product needs to be distilled out, thereby producing a large amount of waste residue; in the prior art, the catalyst of the first step reaction is also used as the catalyst of the second step reaction for direct hydrolysis, although the problem of waste residue is solved, but its yield The efficiency is low, only reaching 91.5%, and the preparation of the catalyst required for the first step reaction is complicated and expensive, and the product still needs to be separated by distillation. The production cost is high, which is not conducive to industrial production
In addition, the above method cannot be prepared continuously, thereby reducing production efficiency

Method used

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  • Synthesis method of 2,4-dichloro-5-fluorobenzoyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Put the industrial grade HZSM-5 molecular sieve in a tube furnace, and raise the temperature to 600°C at a heating rate of 10°C / min. After the temperature is constant, use a peristaltic pump to feed purified water for 1 hour, then dry and cool. Obtain the modified HZSM-5 molecular sieve, which is placed in a sealed bag for subsequent use;

[0026] (2) Put 100g of the above-mentioned modified HZSM-5 molecular sieve into a fixed bed reactor, control the temperature of the bed pass to 100±0.5°C, and feed in equimolar mixed 2,4-dichloro-5-fluorotrichloro Toluene, the liquid hourly space velocity is 0.5h -1 , reacted at normal pressure for 1h, directly obtained 49.9g light yellow liquid from the bottom of the fixed bed reactor, and said light yellow liquid contained 2,4-dichloro-5-fluorobenzoyl chloride, 2,4-dichloro-5- The content of fluorobenzoyl chloride is 98.3%, and the yield is 98.1%.

Embodiment 2

[0028] (1) Put the industrial grade HZSM-5 molecular sieve in a tube furnace, and raise the temperature to 600°C at a heating rate of 10°C / min. After the temperature is constant, use a peristaltic pump to feed purified water for 1 hour, then dry and cool. Obtain the modified HZSM-5 molecular sieve, which is placed in a sealed bag for subsequent use;

[0029] (2) Put 100g of the above-mentioned modified HZSM-5 molecular sieve into a fixed bed reactor, control the temperature of the bed pass to 140±0.5°C, and feed in equimolar mixed 2,4-dichloro-5-fluorotrichloro Toluene, the liquid hourly space velocity is 1.8h -1 , reacted at 0.35MPa for 1h, and directly obtained 179.8g of light yellow liquid from the bottom of the fixed bed reactor, which contained 2,4-dichloro-5-fluorobenzoyl chloride, 2,4-dichloro-5 The content of -fluorobenzoyl chloride is 99.6%, and the yield is 99.5%.

Embodiment 3

[0031] (1) Put the industrial grade HZSM-5 molecular sieve in a tube furnace, and raise the temperature to 600°C at a heating rate of 10°C / min. After the temperature is constant, use a peristaltic pump to feed purified water for 1 hour, then dry and cool. Obtain the modified HZSM-5 molecular sieve, which is placed in a sealed bag for subsequent use;

[0032] (2) Put 100g of the above-mentioned modified HZSM-5 molecular sieve into a fixed bed reactor, control the temperature of the bed pass to 180±0.5°C, and feed in equimolar mixed 2,4-dichloro-5-fluorotrichloro Toluene, the liquid hourly space velocity is 3.0h -1 , reacted for 1h under 1.0MPa, and directly obtained 299.7g light yellow liquid from the bottom of the fixed bed reactor, which contained 2,4-dichloro-5-fluorobenzoyl chloride, 2,4-dichloro-5 The content of -fluorobenzoyl chloride is 98.7%, and the yield is 98.5%.

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Abstract

The invention belongs to the technical field of drug intermediate synthesis and particularly relates to a synthesis method of 2,4-dichloro-5-fluorobenzoyl chloride. The synthesis method comprises the following steps of filling a bed layer of a fixed bed reactor with acidic zeolite; and after premixing 2,4-dichloro-5-fluorobenzotrichloride and water, reacting at the temperature of 100-180 DEG C in a way of flowing through the fixed bed reactor to obtain 2,4-dichloro-5-fluorobenzoyl chloride. According to the synthesis method, 2,4-dichloro-5-fluorobenzoyl chloride is synthesized through catalytic hydrolysis of the acidic zeolite, so that qualified products with the yield of more than 99% can be obtained directly; and distillation separation is not needed in the reaction process, so that the production process is simplified. The bed layer of the fixed bed reactor is filled with the acidic zeolite, so that the problem that a reaction product is separated from a catalyst does not exist, the problems of waste residues and environment pollution do not exist, and therefore, the conflict among production cost, yield and environment pollution is successfully solved.

Description

technical field [0001] The invention belongs to the technical field of synthesis of pharmaceutical intermediates, and in particular relates to a synthesis method of 2,4-dichloro-5-fluorobenzoyl chloride. Background technique [0002] Environmental protection has become a decisive basis for the sustainable development of my country's economy. With the development of my country's economy, environmental issues have always been the focus of attention of the whole country. In the face of frequent natural disasters and repeated pollution accidents, environmental protection must cause enough attention. [0003] 2,4-dichloro-5-fluorobenzoyl chloride is a highly active antibacterial drug intermediate, mainly for the preparation of special antipsychotic drugs such as trihaloperidol, trihaloperidine, penfluridol, quinolones and other drugs It is also used for the identification of pesticides, insecticides, ovicides, plastics, resins, etc., and more of them are used to synthesize broad-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/58C07C63/70B01J29/40
CPCB01J29/40C07C51/58C07C63/70Y02P20/50
Inventor 王伟宏王兴国李承峰赵肖泽张建强孟德伟廖仕学李琦斌杨俊德
Owner SHANDONG GUOBANG PHARMA