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Efficient and green synthesis method of 2, 3, 4, 5-tetrafluorobenzoyl chloride

A technology for tetrafluorobenzoyl chloride and green synthesis, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve the problems of low production yield, achieve increased yield, and increase product yield , The effect of less damage to the reaction material

Pending Publication Date: 2022-04-12
内蒙古源宏精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The whole process involves 5 steps of reaction, and various solvents are used in the production process, and the product can only be obtained after post-treatment in each step, which involves many operations, and the original process uses concentrated sulfuric acid for hydrolysis reaction, concentrated sulfuric acid will make the material Carbonization, producing a lot of tar, low production yield

Method used

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  • Efficient and green synthesis method of 2, 3, 4, 5-tetrafluorobenzoyl chloride
  • Efficient and green synthesis method of 2, 3, 4, 5-tetrafluorobenzoyl chloride
  • Efficient and green synthesis method of 2, 3, 4, 5-tetrafluorobenzoyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Put 200ml of toluene into the reaction kettle, put in 45g of potassium fluoride, 1g of catalyst tetramethylammonium chloride, and 50g of tetrachlorophthalic anhydride, raise the temperature to 100°C, then seal it and raise the temperature to 120-150°C, fill it with nitrogen to 0.4MPa, and carry out Insulate and react for 5 hours, take a sample for liquid chromatography detection, the spectrum shows that the peak purity of tetrachlorophthalic anhydride of the raw material is ≤1%, and then cool down to 50°C for pressure filtration to remove potassium chloride, potassium chloride is dried as a by-product, and the toluene mother liquor is removed Next reaction.

[0023] Transfer the toluene filtrate from the previous step to the decarboxylation reactor, control the temperature at about 45°C, add 18g of water (use 1 batch of water for one layering, add 3.5g of water), 12.5g of sodium carbonate (use 1 batch of sodium carbonate, add new Sodium carbonate 1g), warming up to 75-8...

Embodiment 2

[0026] Put 150ml of toluene into the reaction kettle, put in 50g of potassium fluoride, 1g of catalyst tetramethylammonium chloride, and 50g of tetrachlorophthalic anhydride, raise the temperature to 100°C, then seal it and raise the temperature to 120-150°C, fill it with nitrogen to 0.4MPa, and carry out Insulate and react for 5 hours, take a sample for liquid chromatography detection, the spectrum shows that the peak purity of tetrachlorophthalic anhydride of the raw material is ≤1%, and then cool down to 50°C for pressure filtration to remove potassium chloride, potassium chloride is dried as a by-product, and the toluene mother liquor is removed Next reaction.

[0027] Transfer the toluene filtrate from the previous step to the decarboxylation reaction kettle, control the temperature at about 45°C, add 17g of water (use 1 batch of water for one layering, add 3.0g of water), 12.5g of sodium carbonate (use 1 batch of sodium carbonate, add new Sodium carbonate 1g), warming up...

Embodiment 3

[0030] Put 250ml of toluene into the reaction kettle, put 40g of potassium fluoride, 1g of catalyst tetramethylammonium chloride, and 50g of tetrachlorophthalic anhydride, raise the temperature to 100°C, then seal it and raise the temperature to 120-150°C, fill it with nitrogen to 0.4MPa, and carry out Insulate and react for 5 hours, take a sample for liquid chromatography detection, the spectrum shows that the peak purity of tetrachlorophthalic anhydride of the raw material is ≤1%, and then cool down to 50°C for pressure filtration to remove potassium chloride, potassium chloride is dried as a by-product, and the toluene mother liquor is removed Next reaction.

[0031] Transfer the toluene filtrate from the previous step to the decarboxylation reaction kettle, control the temperature at about 45°C, add 20g of water (use 1 batch of water for one layering, add 4.0g of water), 12.5g of sodium carbonate (use 1 batch of sodium carbonate, add new Sodium carbonate 1g), warming up to...

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Abstract

The invention discloses an efficient and green synthesis method of 2, 3, 4, 5-tetrafluorobenzoyl chloride, which is characterized by comprising the following steps: S1, fluorination; s2, carrying out decarboxylation; and S3, acylating chlorination. According to the invention, tetrachlorophthalic anhydride is mainly used as a raw material, toluene, xylene, chlorobenzene or o-dichlorobenzene is used as a solvent, tetramethylammonium chloride is used as a phase transfer catalyst to react with alkali metal salt potassium fluoride to prepare tetrafluorophthalic anhydride, then a sodium carbonate (or sodium bicarbonate, potassium carbonate or potassium bicarbonate) aqueous solution is added to carry out decarboxylation reaction, and the tetrachlorophthalic anhydride is obtained. After the reaction is finished, standing for layering, removing a water layer for mechanical application, and dropwise adding thionyl chloride into an organic toluene layer for reaction to obtain tetrafluorobenzoyl chloride. In the whole production process, the reaction conversion rate is high, solid waste and the like are basically avoided in the production process, and the method is a green synthesis method.

Description

Technical field: [0001] The invention relates to a synthesis method, in particular to a high-efficiency green synthesis method of 2,3,4,5-tetrafluorobenzoyl chloride. Background technique: [0002] 2,3,4,5-Tetrafluorobenzoyl chloride, formula C 7 HClF 4 O, molecular weight: 212.5289, CAS number: 94695-48-4, density: 1.601g / cm 3 Boiling point: 174.4°C at 760mmHg, flash point: 59.3°C, physical and chemical properties: colorless transparent liquid, is an important pharmaceutical raw material intermediate, the main purpose is to produce levofloxacin. [0003] The industrial synthesis route of 2,3,4,5-tetrafluorobenzoyl chloride is: using phthalic anhydride as raw material, through chlorination, imidization, fluorination, hydrolysis, decarboxylation and acyl chloride reaction to obtain 2,3,4, 5-tetrafluorobenzoyl chloride. In this process, after the chlorination of phthalic anhydride to produce tetrachlorophthalic anhydride, the imidization reaction with the aqueous solution ...

Claims

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Application Information

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IPC IPC(8): C07C51/60C07C63/70
CPCY02P20/584
Inventor 王兵波张森王伟张晓弟宋立雪
Owner 内蒙古源宏精细化工有限公司
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