In-tank type electrochemical synthesizing method of p-methoxy phenylacetone

A technology of methoxyphenylacetone and a synthesis method, applied in the field of electrochemistry, can solve the problems of many operation steps, low yield, long synthesis route and the like, and achieves the advantages of simple and easy-to-obtain reaction raw materials, simple and safe operation, and pollution avoidance. Effect

Inactive Publication Date: 2005-12-21
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] 1. British Patent No.1119612 uses peracetic acid to oxidize 1-(4-methoxyphenyl)propylene, and the oxidation product uses acidic substances such as ZnCl 2 After the reaction, p-methoxyphenylacetone is obtained. The disadvantage is that the yield in the acid treatment process is low, and the raw material peroxygen compound is easy to explode, and the operation must be extremely careful
[0005] 2. U.S. JACS, 77,700 (1955) uses 4-methoxyphenylacetonitrile to react with sodium ethoxide in ethyl acetate to obtain a precursor compound containing an acetyl group, which is then hydrolyzed to obtain p-methoxyphenylacetone. The disadvantage is Due to the use of sodium ethoxide, the entire reaction system must strictly remove water, and the yield of the hydrolysis step is low, and the preparation has to add the step of synthesizing the raw material 4-methoxyphenylacetonitrile, the synthesis route is long, and the operation steps are many
[0006] 3. U.S. Patent No. 4,638,094 utilizes 3-(4-methoxyphenyl)propene and a

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] In the second step, 20g acetic acid: the volume ratio of acetic anhydride is 1: 1 acetic acid-: acetic anhydride solvent, 1g potassium acetate and 5g lead acetate are mixed, refluxed 6 hours under 80 ℃, obtain anolyte, inject described anode Chamber, 20g acetic acid: the volume ratio of acetic anhydride is 1: 1 acetic acid-: acetic anhydride solvent and 5g potassium acetate are mixed, refluxed 6 hours under 80 ℃, obtain catholyte, inject described cathode chamber;

[0035] In the third step, the amount of anethole added is 0.4g, the temperature is 20°C, and the current density is 15mA / cm 2 , power supply 5.4×10 -3 F;

[0036] In the 4th step, under 60 ℃, 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 20%;

[0037] In the fifth step, the product was obtained, p-methoxyphenylacetone 0.31g;

[0038] In the sixth step, lead acetate is recycled.

[0039] In the fifth step...

Embodiment 2

[0041] In the second step, 20g acetic acid: the volume ratio of acetic anhydride is 1: 1 acetic acid-: acetic anhydride solvent, 3g potassium acetate and 3g lead acetate mix, reflux 6 hours under 80 ℃, obtain anolyte, inject described anode Chamber, all the other are with the second step of embodiment 1;

[0042] In the third step, the amount of anethole added is 0.4g, the temperature is 50°C, and the current density is 10mA / cm 2 , the current flow is 5.4×1 0 -3 F;

[0043] In the fourth step, hydrolysis at 80°C for 6.5 hours, H 2 SO 4 The concentration of the solution is 40%;

[0044] In the fifth step, the product is obtained, p-methoxyphenylacetone 0.35g;

[0045] In the sixth step, lead acetate is recycled.

[0046] In the fifth step, the yield was 88.0%.

Embodiment 3

[0048] In the second step, 20g acetic acid: the volume ratio of acetic anhydride is 1: 1 acetic acid-: acetic anhydride solvent, 5g potassium acetate and 1g lead acetate mix, reflux 6 hours under 80 ℃, obtain anolyte, inject described anode Chamber, all the other are identical with the second step of embodiment 1 with the second step of embodiment 1;

[0049] In the third step, the amount of anethole added is 0.4g, the temperature is 80°C, and the current density is 5mA / cm 2 , power supply 5.4×10 -3 F;

[0050] In the fourth step, hydrolysis at 100°C for 3 hours, H 2 SO 4 The concentration of the solution is 60%;

[0051] In the fifth step, the product was obtained, p-methoxyphenylacetone 0.34g;

[0052] In the sixth step, lead acetate is recycled.

[0053] In the fifth step, the yield was 85.7%.

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Abstract

The invention discloses a tank-interior electrochemistry composite technique of methoxylbenzyl-ketone relates to electrochemistry technique field. Adopt Pt filament as positive pole and stainless fin as negative pole in bi-room electrolysis tank, acetic acid-acetic acid anhydride as disslovant, kalium acetate as electrolysis support, at certain temperature, in the electrolysis tank in positive pole room the anethole and lead acetate both as electrolysis basal material. The anethole directly electrolysis reaction on the positive pole takes place at the same time the indirect oxidation with lead tertraacetic as intermediate reactor develops. Hydrolyric decomposite the obtained product with sulfuric acid and further process to acquire the final product methoxylbenzyl-ketone. The invention has got advantages such as simple and easy reaction material, environmental reaction process, safe operation, high productivity and low cost, is a technique of high added value.

Description

technical field [0001] The invention relates to an in-tank electrochemical synthesis method of p-methoxyphenylacetone, which belongs to the technical field of electrochemistry. Background technique [0002] p-methoxyphenylacetone, molecular formula C 10 h 12 o 2 , with a boiling point of 266-268°C and a relative density of 1.067, it is an important synthetic intermediate for pesticides, medicines, especially synthetic antihypertensive drugs, antidepressants, etc., such as 4-methoxy-N-methyl prepared from it as an intermediate - Amphetamines are used as central nervous system stimulants in the treatment of narcolepsy and depression and are now widely used in Europe. [0003] Although p-methoxyphenylacetone is a very useful intermediate, a very satisfactory preparation process has not been found so far in actual industrial production. [0004] 1. British Patent No.1119612 uses peracetic acid to oxidize 1-(4-methoxyphenyl)propylene, and the oxidation produ...

Claims

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Application Information

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IPC IPC(8): C25B3/23
Inventor 陆嘉星叶小鹤王欢张爱建薛腾
Owner EAST CHINA NORMAL UNIV
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