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A kind of synthetic method of 2,4-dichloro-5-fluorobenzoyl chloride

A technology for the synthesis of fluorobenzoyl chloride and its synthesis method, which is applied in the field of synthesis of fine chemical intermediates, which can solve the problems of the use of highly toxic chemicals, excessively long process routes, and high equipment requirements, and achieve less pollutant discharge, short process routes, and high production efficiency. good safety effect

Active Publication Date: 2021-11-09
ZHEJIANG BENLI TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0035] The purpose of the present invention is to provide a brand-new synthetic method of 2,4-dichloro-5-fluorobenzoyl chloride, which solves the problem of excessively long process route, cumbersome aftertreatment, high equipment requirements and highly toxic chemicals in the prior art. The use, low yield, poor quality and other problems that are not suitable for industrial production

Method used

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  • A kind of synthetic method of 2,4-dichloro-5-fluorobenzoyl chloride
  • A kind of synthetic method of 2,4-dichloro-5-fluorobenzoyl chloride
  • A kind of synthetic method of 2,4-dichloro-5-fluorobenzoyl chloride

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Embodiment 1-1

[0066] Treat the cationic resin with 1mol / L sodium hydroxide first, then wash it with hydrochloric acid, wash it with water until it is neutral, and then immerse it in 0.5mol / L FeCl 3 Stir in the solution for 8 hours, then slowly add HF until the pH is 2 to 3; age the reaction system at -5°C for 24 hours, filter and wash with suction, then dry the filter cake at 80°C to obtain a cationic resin Catalyst (ie catalyst Cat.1).

Embodiment 2-1

[0069] Add 165g (1mol) of 2,4-dichlorofluorobenzene and 0.77g of Cat. 2 to 2MPa, stirred and reacted for 3 hours to obtain a reaction solution; then add CCl dropwise to the reaction solution 4 15.4g (0.1mol), heat up to 60°C, keep warm for 2 hours, the hydrogen chloride generated by the reaction is absorbed by falling film, after the reaction, the material obtained by the reaction is filtered to recover the catalyst Cat.1, and the filtrate is distilled under reduced pressure to obtain 2 , 44.95g of 4-dichloro-5-fluorobenzoyl chloride, yield 98.8%.

Embodiment 2-2

[0071] Add 330g (2mol) of 2,4-dichlorofluorobenzene and 1.54g of catalyst Cat.1 into the reaction flask, first raise the temperature to 40°C, and then introduce 2 to 2MPa, stirred and reacted for 4 hours to obtain a reaction solution; then add CCl dropwise to the reaction solution 4 15.4g (0.1mol), heat up to 60°C, keep warm for 2 hours, the hydrogen chloride generated by the reaction is absorbed by falling film, after the reaction, the material obtained by the reaction is filtered to recover the catalyst Cat.1, and the filtrate is distilled under reduced pressure to obtain 2 , 44.8g of 4-dichloro-5-fluorobenzoyl chloride, yield 98.5%.

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Abstract

The invention relates to a synthesis method of quinolone drug intermediate 2,4-dichloro-5-fluorobenzoyl chloride. The synthesis method includes: preparing 2,4-dichloro-5-fluorobenzoyl chloride from 2,4-dichlorofluorobenzene, carbon dioxide and carbon tetrachloride under the action of a cationic resin catalyst. The invention solves the problems in the prior art that the process route is too long, the post-processing is complicated, the equipment requirements are high, the use of highly toxic chemicals, the yield is low, the quality is poor, etc. and are not suitable for industrial production. The beneficial effects are as follows: raw materials are cheap and easy to obtain, the process route is short, production safety is good, the catalyst is easy to separate, waste acid emissions are low, post-processing is simple, the yield is high, the quality is good, and it is suitable for industrial continuous production.

Description

technical field [0001] The invention relates to the technical field of synthesis of fine chemical intermediates, in particular to a synthesis method of quinolone drug intermediate 2,4-dichloro-5-fluorobenzoyl chloride. Background technique [0002] 2,4-Dichloro-5-fluorobenzoyl chloride, CAS number 86393-34-2, molecular formula C 7 h 2 Cl 3 FO, the chemical structural formula is as follows: [0003] [0004] The compound is the main raw material for the preparation of antipsychotic specific drugs triflupiperidinol, trifluoropiperidinol, penfluridol and synthetic broad-spectrum antibiotics such as ciprofloxacin and other third-generation quinolones, and can also be used for pesticide killing Insecticides and ovicides, etc., and the identification of plastics and resins. 2,4-dichloro-5-fluorobenzoyl chloride is also an important basic raw material for the synthesis of high-performance new polymer materials polyaryl ketones, polyaryl ketones are a class of semi-crystallin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/58C07C63/70
CPCC07C51/58C07C63/70
Inventor 顾海宁吴政杰余永志徐洪顺
Owner ZHEJIANG BENLI TECH CO LTD
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