3-fluorocinnamic acid synthesis method
A technique for the synthesis of m-fluorocinnamic acid and its synthesis method, which is applied in the field of synthesis of m-fluorocinnamic acid, can solve the problems of low purity of the crude product, large amount of solvent pyridine used, and long reaction time, etc., so as to reduce the amount of solvent and catalyst used, shorten Synthesis reaction time, effect of optimized post-treatment process
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Embodiment 1
[0014] Add 31g of m-fluorobenzaldehyde and 3.3g of pyridine into a four-necked flask, stir and heat to 90°C, stir and add 31.25g of malonic acid in 5 batches until it is completely dissolved, after adding malonic acid, raise the temperature to 110°C and stir Reflux for 90min. Add 75mL of 10% hydrochloric acid into the four-necked flask, and cool to room temperature. Suction filter, and wash the solid with hot water above 70°C until the pH of the washing liquid is neutral and the washing liquid is colorless. The solid was dried to obtain white flaky crystals with a yield of 79.5%.
Embodiment 2
[0016] Add 31g of m-fluorobenzaldehyde and 6.59g of pyridine into a four-neck flask, stir and heat to 90°C, stir and add 31.25g of malonic acid in 5 batches until it is completely dissolved, after adding malonic acid, raise the temperature to 110°C and stir Reflux for 120min. Add 75mL of 10% hydrochloric acid into the four-necked flask, and cool to room temperature. Suction filter, and wash the solid with hot water above 70°C until the pH of the washing liquid is neutral and the washing liquid is colorless. The solid was dried to obtain white flaky crystals with a yield of 85.5%.
Embodiment 3
[0018] Add 31g of m-fluorobenzaldehyde and 9.89g of pyridine into a four-neck flask, stir and heat to 90°C, stir and add 31.25g of malonic acid in 5 batches until it is completely dissolved, after adding malonic acid, raise the temperature to 110°C and stir Reflux for 150min. Add 85mL of 10% hydrochloric acid to the four-neck flask, and cool to room temperature. Suction filter, and wash the solid with hot water above 70°C until the pH of the washing liquid is neutral and the washing liquid is colorless. The solid was dried to obtain white flaky crystals with a yield of 74.7%.
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