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A highly stable and reusable Cu NP cathode was prepared for the electrosynthesis of cyclic carbonates from CO2 and epoxides under mild conditions.

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The electrogenerated cyanomethyl anion reacts with diols in the presence of CO2 to yield the corresponding cyclic carbonates in moderated yields. The reported methodology has been carried out under mild conditions, avoiding any addition of classical bases, catalysts. In this communication, the effects of reaction conditions – such as supporting electrolyte, cathode material, current densities, charge amount, diol concentration – have been investigated to optimize the carbonates yield. © 2011 Society of Chemical Industry and John Wiley & Sons, Ltd

In the one compartment electrochemical cell 2-hydroxy-2-p-tolyl-butyric acid methyl ester was electrosynthesized by electrochemical carboxylation of p-methylpropiophenone in the presence of carbon dioxide. Under galvanostatic conditions, the electrocarboxylation was influenced by supporting electrolytes, cathode materials, the current density, passed charge and temperatures. Application scope of the eletrocarboxylation system was then examined, and an excellent yield of 97% was obtained when the electrolysis was carried out in DMF-0.1 mol•L -1TEABr solution using cheap and environmentally benign nickel as the cathode under a controlled current density of 5.0 mA•cm -2 until 2.8 F•mol -1 charge passed through the cell at -10 ℃. The electrochemical behavior of p-methoxylacetophenone has been studied on the glassy carbon electrode by cyclic voltammetry and the probable mechanism was proposed accordingly.

An active catalyst, [Cu]@Ag composite, was synthesized for the first time and used as a cathode for electrocarboxylation of cinnamyl chloride with CO 2 . b,g-Unsaturated carboxylic acids were obtained with excellent yield and moderate selectivity. Moreover, reasonable yields and selectivities of carboxylic acids were also achieved with several allylic halides and aryl halides.Scheme 1 Regiodivergency in allyl electrophiles and our concept of the allylation of CO 2 .

A simple and efficient electrocatalytic carboxylation of benzyl chloride with CO 2 is described. The reaction operates under 1 atm CO 2 and room temperature in a single chamber electrolysis cell with Cu foam cathode and Mg sacrificial anode. No additional catalyst is needed, and noble metal is not necessary. The effects of cathode material, solvent current density, charge amount, and temperature were studied using 1-phenylethyl chloride as a model compound. Under optimal conditions, 99% yield of 2-phenylpropionic acid could be obtained. Moreover, reasonable yields were also achieved with other benzyl chlorides.