A green production process for 2,4-dichloro-5-fluorobenzoyl chloride
A technology of fluorobenzoyl chloride and dichlorofluorobenzene, which is applied in the chemical field, can solve the problems of low utilization rate of raw materials, large pollution, immature by-product dimer conversion process, etc., and achieves increased production cost, reduced production cost, The effect of avoiding the formation of a large number of by-products
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Embodiment 1-4
[0052] Add 33g of 2,4-dichlorofluorobenzene into 30.8g of carbon tetrachloride, stir to dissolve, add 65.8g of aluminum trichloride, raise the temperature to 40°C and maintain it for 8 hours, the reaction is complete, and compound I and compound II are obtained. After hydrolysis and distillation, 2,4-dichloro-5-fluorobenzoyl chloride and compound III were obtained;
[0053] Add 10 g of ethanol, 25 g of 2,4-dichlorofluorobenzene, and different masses of tetrabutylammonium chloride into the flask, and then add 12.5 g of compound III and 3 g of sodium hydroxide. Raise the temperature to 110°C and react for 3 hours, control compound III to less than 0.2%, recover ethanol and part of 2,4-dichlorofluorobenzene for use. After the recovery is complete, add water, remove the lower layer, and rectify the lower layer under reduced pressure to obtain 2,4-dichlorofluorobenzene. After separation, the pH was adjusted to 1 with hydrochloric acid. After the adjustment, compound Ⅴ precipitate...
Embodiment 5-8
[0056] Add 33g of 2,4-dichlorofluorobenzene into 30.8g of carbon tetrachloride, stir to dissolve, add 65.8g of aluminum trichloride / solid acid composite catalyst, raise the temperature to 40°C and maintain it for 8 hours, the reaction is complete, and the compound is obtained I and compound II are separated by distillation after hydrolysis to obtain 2,4-dichloro-5-fluorobenzoyl chloride and compound III;
[0057] 10 g of ethanol, 25 g of 2,4-dichlorofluorobenzene and 0.125 g of tetrabutylammonium chloride were added to the flask, and then 12.5 g of compound III and 3 g of sodium hydroxide were added. Raise to temperature T1 and react for 3 hours, control compound III to less than 0.2%, recover ethanol and part of 2,4-dichlorofluorobenzene for use. After the recovery is complete, add water, remove the lower layer, and rectify the lower layer under reduced pressure to obtain 2,4-dichlorofluorobenzene. After separation, the pH was adjusted to 1 with hydrochloric acid. After the...
Embodiment 9
[0061] Add 33g of 2,4-dichlorofluorobenzene into 30.8g of carbon tetrachloride, stir to dissolve, add 65.8g of aluminum trichloride / mordenite composite catalyst, raise the temperature to 40°C and maintain it for 8 hours, the reaction is complete, and the compound is obtained I and compound II are separated by distillation after hydrolysis to obtain 2,4-dichloro-5-fluorobenzoyl chloride and compound III;
[0062] 10 g of ethanol, 25 g of 2,4-dichlorofluorobenzene and 0.125 g of tetrabutylammonium bromide were added to the flask, and then 12.5 g of compound III and 3 g of sodium hydroxide were added. Raise the temperature to 110°C and react for 3 hours, control compound III to less than 0.2%, recover ethanol and part of 2,4-dichlorofluorobenzene for use. After the recovery is complete, add water, remove the lower layer, and rectify the lower layer under reduced pressure to obtain 2,4-dichlorofluorobenzene. After separation, the pH was adjusted to 1 with hydrochloric acid. Afte...
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