A Facile and Economic Preparation of Deuterated Chloroform for Laboratory‐Scale

Deuterated chloroform (CDCl 3 ) is a widely used solvent for nuclear magnetic resonance (NMR) spectroscopy in research and academic settings. Existing preparation methods employing catalysts such as hypochlorite salts, pyridine, polyvinylpyridine, catalytic complexes, and polyvinylimidazole often face limitations in yield, scalability, or environmental sustainability. This study presents a practical laboratory‐scale one‐pot synthesis employing hexachloroacetone (HCA) and deuterium oxide (D 2 O), with imidazole as the primary base catalyst, alongside a comparative evaluation of other nitrogen‐containing base catalysts, including 4‐dimethylaminopyridine (DMAP), benzimidazole, 1,4‐diazabicyclo[2.2.2]octane (DABCO), and indole. This process involves the reduction and decarboxylation of HCA, offering high chemical yield, high isotopic yield, cost‐effectiveness, and ease of synthesis. Among the evaluated base catalysts, imidazole provides notable advantages, including stability and solubility in D 2 O, enabling cleaner, more sustainable reactions. Hence, this newer method is suitable for research laboratories and undergraduate teaching, with potential benefits in reducing solvent costs and promoting greener chemistry practices.