One-room type electrochemical synthesis method for alpha-phenylacetpropionic acid

Abstract

The invention relates to a one-compartment electrochemical synthesis method for alpha-phenyl-levulinic acids, belonging to the electrochemistry technical field. In a one-compartment electrolytic cell, a magnesium rod is used as an anode; a stainless sheet steel is used as a cathode; Ag / AgI is used as a reference electrode; acetonitrile is used as solvent; tetraethyl tetra-ammonium fluoroborate is used as supporting electrolytes; benzalacetone is used as electrolytic reaction substrates; constant electric potential electrolysis is performed under the condition of normal atmosphere CO2, different temperatures and different electrolytic electric potentials; after electrolysis is stopped, the reaction mixture is acidified by 2 mol / L HCl; after extraction of ethers, an ether layer is washed by NaOH until the water layer is alkaline; HC1 is then added into the water layer until the water layer is acidic; after extraction of the ethers, the ether layer is washed by saturated NaC1 water solution and then dried by anhydrous MgSO4; after revolving evaporation, the alpha-phenyl-levulinic acids are obtained. The method has the advantages of easy acquisition of reaction raw materials, inexpensive price, greenness of the reaction process, simple, convenient and safe operation, high yield and low cost and is a technological line with high added value.

Description

technical field [0001] The invention relates to a one-chamber electrochemical synthesis method of α-phenyl-levulinic acid, which belongs to the technical field of electrochemistry. Background technique [0002] α-Phenyl-levulinic acid, formula C 11 h 12 o 3 , melting point 126 ° C, α-phenyl-levulinic acid is a γ-keto acid, is a very useful organic synthesis raw materials and intermediates, widely used in the synthesis of various lactones, heterocyclic compounds and other aspects. [0003] Although α-phenyl-levulinic acid is a very useful intermediate, a very satisfactory preparation process has not been found so far in actual industrial production. [0004] 1. Heating β-ketoamine with KCN or NaCN aqueous solution can generate cyano compound, which can be obtained by hydrolysis. The disadvantage is that the raw materials and intermediates are highly toxic, seriously pollute the environment, and are not conducive to industrial production. [0005] 2. Ethyl acetoacetate an...

AI Technical Summary

Problems solved by technology

The disadvantage is that due to the use of mercury electrodes, the environmental pollution is serious; the electrolytic cell is a two-chamber type, and the production cost increases

[0008] In recent years, there have been no reports on the synthesis of α-phenyl-levulinic acid by an environmentally friendly and "green" electrochemical method at home and abroad.