Preparation method of 2,3,4,5-tetrafluorobenzoyl chloride
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 complicated operation process, long production cycle, and many product losses, etc., To achieve the effect of simplifying the operation process, reducing production time and avoiding product loss
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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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