Out of tank type electrochemical synthesizing method of p-methoxy phenylacetone
A kind of technology of methoxyphenylacetone and synthesis method, applied in the field of electrochemistry, can solve the problems of many operation steps, low yield, long synthesis route, etc., and achieve simple and easy-to-obtain reaction raw materials, simple and safe operation, and avoid pollution Effect
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Embodiment 1
[0034] In the second step, 20g acetic acid: the volume ratio of acetic anhydride is 1: acetic acid-: acetic anhydride solvent, 1g potassium acetate are supporting electrolyte and 5g lead acetate mix, reflux 6 hours under 80 ℃, obtain anolyte, inject institute Described anode compartment, 20g acetic acid: the volume ratio of acetic anhydride is 1: 1 acetic acid-: acetic anhydride solvent and 5g potassium acetate are supporting electrolyte mix, reflux 6 hours under 80 ℃, obtain catholyte, inject described cathode room;
[0035] In the third step, at 20°C, the current density is 5mA / cm 2 , power supply 5.4×10 -3 F, after stopping the electrolysis, add the electrolyte solution containing lead tetraacetate in the anode chamber to 0.4g anethole at normal pressure and 40°C, and react for 30 hours;
[0036] In the 4th step, under 100 ℃, hydrolyze for 10 hours, the addition of water is 20g, the consumption of diethyl ether is each 10g, H 2 SO 4 The concentration of the solution is ...
Embodiment 2
[0041] In the second step, 20g acetic acid: the volume ratio of acetic anhydride is 1: acetic acid-: acetic anhydride solvent, 3g potassium acetate are supporting electrolyte and 3g lead acetate mix, reflux 6 hours under 80 ℃, obtain anolyte, inject all Described anode chamber, all the other are with the second step of embodiment 1;
[0042] In the third step, at 40°C, the current density is 10mA / cm 2 , power supply 5.4×10 -3 F, after stopping the electrolysis, add the electrolyte solution containing lead tetraacetate in the anode chamber to 0.4g anethole at normal pressure and 60°C, and react for 20 hours;
[0043] In the fourth step, hydrolyze at 80°C for 7 hours, H 2 SO 4 The concentration of the solution is 40%;
[0044] In the fifth step, the product was obtained, p-methoxyphenylacetone 0.247g;
[0045] In the sixth step, lead acetate is recycled.
[0046] In the fifth step, the yield was 61.9%.
Embodiment 3
[0048] In the second step, 20g acetic acid: the volume ratio of acetic anhydride is 1: acetic acid-: acetic anhydride solvent, 5g potassium acetate are supporting electrolyte and 1g lead acetate mix, reflux 6 hours under 80 ℃, obtain anolyte, inject institute Described anode chamber, all the other are with the second step of embodiment 1;
[0049] In the third step, at 60°C, the current density is 15mA / cm 2 , power supply 5.4×10 -3 F, after stopping the electrolysis, add the electrolyte solution containing lead tetraacetate in the anode chamber to 0.4g anethole at normal pressure and 80°C, and react for 10 hours;
[0050] In the fourth step, hydrolysis at 60°C for 10 hours, H 2 SO 4The concentration of the solution is 60%;
[0051] In the fifth step, the product was obtained, p-methoxyphenylacetone 0.21g;
[0052] In the sixth step, lead acetate is recycled.
[0053] In the fifth step, the yield was 52.8%.
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