Preparation method of 2,3,4,5-tetrafluorobenzoyl chloride
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A technology of tetrafluorobenzoyl chloride and tetrafluorobenzoic acid is applied in the field of preparation of 2,3,4,5-tetrafluorobenzoyl chloride, and can solve the problems of cumbersome operation process, high product loss, troublesome solvent recovery and application, etc. , to achieve the effect of simplifying the operation process, avoiding product loss and shortening the production cycle
Active Publication Date: 2015-03-04
ZHEJIANG ZHONGXIN FLUORIDE MATERIALS CO LTD
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Problems solved by technology
The above-mentioned preparation process has cumbersome operation process, troublesome solvent recovery and application, long production cycle, high energy consumption, low production efficiency, and more product loss in the post-processing process, which greatly restricts2,3,4,5 -Increasing production and reducing consumption of tetrafluorobenzoyl chloride
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Embodiment 1
[0028] Add 47.6 grams of 3,4,5,6-tetrafluorophthalic acid (I), 285 grams of trimethylbenzene, and 1.5 grams of tri-n-propylamine into a 500 mL three-necked flask equipped with mechanical stirring, a thermometer, and a condenser, and stir to raise the temperature to 150 o C, reacted for 15 hours, and the reaction system was cooled to 20-30 o C, filtered to obtain 39.5 g of crude 2,3,4,5-tetrafluorobenzoic acid (II), and the filtrate was used for the next batch of decarboxylation reaction.
Embodiment 2
[0030] Add 47.6 grams of 3,4,5,6-tetrafluorophthalic acid (I) and 1.5 grams of tri-n-propylamine into a 500 mL three-necked flask equipped with mechanical stirring, a thermometer, and a condenser, and add the recovered Trimethylbenzene, and add trimethylbenzene to 285 grams, stir and heat up to 150 o C, reacted for 15 hours, and the reaction system was cooled to 20-30 o C, filtered to obtain 42.2 g of crude 2,3,4,5-tetrafluorobenzoic acid (II), and the filtrate was used for the next batch of decarboxylation reaction.
Embodiment 3
[0032] Add 35.7 grams of 3,4,5,6-tetrafluorophthalic acid (I), 320 grams of xylene, and 1.5 grams of tri-n-butylamine into a 500 mL three-neck flask equipped with mechanical stirring, a thermometer, and a condenser, and stir Warm up to 135 o C, reacted for 22 hours, and the reaction system was cooled to 20-30 o C, filtered to obtain 30.3 g of 2,3,4,5-tetrafluorobenzoic acid (II), and the filtrate was used for the next batch of decarboxylation reaction.
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Abstract
The invention discloses a preparation method of 2,3,4,5-tetrafluorobenzoyl chloride, belonging to the technical field of chemical synthesis. The preparation method comprises the following step: performing a reaction of a raw material 3,4,5,6-tetrafluorophthalic acid in a solvent of aromatic hydrocarbon in the presence of a catalytic amount of organic tertiary amine at a temperature of 120-160 DEG C until the content of the raw material is less than 1%, cooling the reaction system to 20-30 DEG C, filtering, wherein an obtained filtrate is used for a next batch of decarboxylic reaction, adding an acyl chlorination reagent and an organic amide catalyst into the filtered solid of 2,3,4,5-tetrafluorobenzoic acid, heating and reacting until the content of 2,3,4,5-tetrafluorobenzoic acid is less than 0.5%, evaporating and removing low-boiling-point substances of the reaction system, and preforming rectification under vacuum to obtain the finished product of 2,3,4,5-tetrafluorobenzoyl chloride. The preparation method disclosed by the invention has the advantages of being simple in steps, high in production efficiency and synthetic efficiency and the like.
Description
Technical field: [0001] The present invention relates to a kind of preparation method of 2,3,4,5-tetrafluorobenzoyl chloride, specifically, relate to a kind of preparation method of 2,3,4 by 3,4,5,6-tetrafluorophthalic acid , The method for 5-tetrafluorobenzoyl chloride belongs to the technical field of chemical synthesis. Background technique: [0002] 2,3,4,5-Tetrafluorobenzoyl chloride is an important pharmaceutical intermediate, widely used in the synthesis of third-generation fluoroquinolone antibacterial drugs, such as (left) ofloxacin, sparfloxacin , Lomefloxacin, Fleroxacin, etc., have broad market prospects. [0003] The industrial synthesis of 2,3,4,5-tetrafluorobenzoyl chloride mainly contains the following two routes: 1, using phthalonitrile as raw material, through chlorination, fluorination, hydrolysis, decarboxylation and acyl chloride reaction, to obtain 2 ,3,4,5-Tetrafluorobenzoyl chloride; 2. Using phthalic anhydride as raw material, through c...
Claims
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