Synthetic method of methyl 3, 4-dimethoxybenzoate
A technology of methyl dimethoxybenzoate and a synthesis method, which is applied in the field of synthesis of methyl 3,4-dimethoxybenzoate, can solve the problems of unfavorable industrial production, poor safety, and high reaction temperature, and can reduce the The effect of three wastes, reducing dosage and high yield
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[0023] The invention provides a kind of synthetic method of 3,4-dimethoxymethyl benzoate, comprising the following steps:
[0024] Under the catalysis of dicyclohexylcarbodiimide, the veratric acid and methanol are subjected to an esterification reaction to obtain methyl 3,4-dimethoxybenzoate; the temperature of the esterification reaction is below 45°C.
[0025] In the present invention, the preparation method of described veratronic acid preferably comprises the following steps:
[0026] Mix veratraldehyde, water, liquid caustic soda and hydrogen peroxide for oxidation reaction to obtain veratronic acid.
[0027] In the present invention, the concentration of described liquid caustic soda is preferably 30wt%, and described hydrogen peroxide is preferably used in the form of hydrogen peroxide, and the concentration of described hydrogen peroxide is preferably 27wt%; The consumption of described veratraldehyde, liquid caustic soda and hydrogen peroxide The ratio is preferably...
Embodiment 1
[0036] Add 500g of water and 60g of veratraldehyde into a clean, odor-free flask, heat to 40°C, stir until all the raw materials are dissolved, then add 60mL of 30% liquid caustic soda, stir for 15min, then slowly add 180mL of hydrogen peroxide dropwise to control the temperature At 30~35°C, the temperature will rise during the dropwise addition, and the dropwise addition will be completed within 3 hours. Stir for 30 minutes, then raise the temperature to 55°C, keep it warm for 2 hours, then raise the temperature to 60°C and keep it for 3 hours, take a sample for testing, after passing the test, lower the temperature to 25°C, add water and hydrochloric acid to adjust the pH to 2, and finally filter, wash and dry to obtain veratric acid .
Embodiment 2
[0038] Add 2000g of dichloromethane to the flask, add 500g of veratronic acid and 132g of methanol (the molar ratio of veratronic acid:methanol is 1:1.5), stir for 30min, add 680g of DCC (dicyclohexylcarbodiimide), and then raise the temperature To 30°C, keep warm for 3 hours and take a sample for detection. After passing the test, lower the temperature to 15°C-25°C, add 200g of water and stir for 30min, then press filter to remove DCU, then wash the organic phase with 200g of water once, and evaporate the solvent to obtain the target product 3. 522.3g of methyl 4-dimethoxybenzoate, yield 97.0%, the solvent is recycled, and the DCU is returned to the factory for recycling.
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