Abstract Nonafluorobutanesulfonyl azide is a shelf-stable, cost-effective and general diazo transfer reagent for the efficient synthesis of α-diazo carbonyl compounds in excellent yields and in very short reaction times, under mild conditions. The diazo products can be readily isolated in pure form after a simple aqueous extractive work-up that avoids chromatographic purification in most cases. Because of its high efficiency and wide substrate scope, shelf- ...