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

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...

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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 alkyl nitrite to react, and simultaneously adds alcohol, palladium catalyst and amine or copper compound in the reaction system, and then carries out the above-mentioned product The final product is obtained by the hydrolysis reaction, and the yield is high, but the composition of the reaction system is complex and the catalyst is expensive

[0007] 4. French patent FR1,450,200 uses 4-methoxybenzaldehyde and α-chloropropionate to react under strong alkali conditions, and then the product is treated under strong acid conditions to obtain p-methoxyphenylacetone. The disadvantage is that the raw material 4 -Methoxybenzaldehyde and α-chloropropionate are expensive and difficult to obtain

[0008] 5. U.S. Patent No. 4,967,009 uses 2-(4-methoxyphenyl)propene and iodosobenzene diacetate to react in glacial acetic acid to obtain p-methoxyphenylacetone. The disadvantage is that the yield is low

[0009] At present, there is no report on the synthesis of p-methoxyphenylacetone by electrochemical method both at home and abroad