# Simple and Scalable Electrochemical Reduction of Alkyl Oxalates Using Carbon‐Based Electrodes

## TL;DR

A new electrochemical method for reducing alkyl oxalates is developed, offering scalability and avoiding harmful reagents.

## Contribution

A scalable, metal-free electrochemical method for alkyl oxalate reduction using carbon electrodes is introduced.

## Key findings

- The method achieves up to 97% yield for 14 ester examples.
- Scale-up experiments up to 120 mmol confirm practical industrial potential.
- Direct distillation and reusable electrodes simplify isolation and application.

## Abstract

In this study, a simple and robustly scalable electrochemical method for the reduction of alkyl oxalates was established. The use of electricity as a universal agent for reduction applications avoids the stoichiometric formation of reagent waste and the use of transition metal catalysts. In addition, employing readily available carbon electrode materials like glassy carbon or graphite provide important prerequisites for later technical applications. This goes along with common solvents such as acetonitrile and acetic acid in combination with a flow electrolysis setup, allowing easy scalability. The scale‐up experiments on up to a 120 mmol scale proved the practical relevance of the method and the potential use for industrial large‐scale synthesis. The method is suitable for a variety of esters, 14 examples up to 97% yield, and the simple deuterium incorporation to obtain highly deuterated alkyl glycolates.

A method for the electrochemical reduction of alkyl oxalates under mild and ambient conditions in a very simple two‐electrode undivided setup under galvanostatic conditions is established. A simple isolation by direct distillation of the crude mixture in combination with the reusability of the electrodes provides all prerequisites for potential technical applications.© 2026 WILEY‐VCH GmbH